Category: 123-90-0

123-90-0, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route., 123-90-0

9.98 g of thiomorpholine and 14.8 g of triflic anhydride were stirred together in DCM at room temperature for 2 hours. The reaction was then partitioned between 1 M K2C03 (aq) and DCM. The organic layer was separated and dried by passing through a hydrophobic frit, then concentrated in vacuo. 13.82 g of the resultant oil was stirred with 85.2 g of oxone in 50 mL of methanol and 50 mL of water for 18 h at room temperature. The reaction was then filtered and washed with methanol and the filtrate concentrated. This was then partitioned between water and EtOAc and the aqueous layer washed 3 times with EtOAc. The combined organic extracts were then dried (MgS04) and concentrated to produce a white solid. This was then stirred at room temperature with 40 g of K2C03 in 80 mL of methanol for 18 h. The methanol was then removed in vacuo and the remains partitioned between DCM and sat. K2CO3 (aq). The combined organic extracts were passed through a hydrophobic frit and concentrated in vacuo to produce the title compound, 3.51 g.

The chemical industry reduces the impact on the environment during synthesis, 123-90-0, I believe this compound will play a more active role in future production and life.

Reference£º
Patent; ARROW THERAPEUTICS LIMITED; WO2005/89771; (2005); A1;,
Thiomorpholine – Wikipedia
Thiomorpholine | C4H9NS – PubChem

123-90-0, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route., 123-90-0

9.98 g of thiomorpholine and 14.8 g of triflic anhydride were stirred together in DCM at room temperature for 2 hours. The reaction was then partitioned between 1 M K2C03 (aq) and DCM. The organic layer was separated and dried by passing through a hydrophobic frit, then concentrated in vacuo. 13.82 g of the resultant oil was stirred with 85.2 g of oxone in 50 mL of methanol and 50 mL of water for 18 h at room temperature. The reaction was then filtered and washed with methanol and the filtrate concentrated. This was then partitioned between water and EtOAc and the aqueous layer washed 3 times with EtOAc. The combined organic extracts were then dried (MgS04) and concentrated to produce a white solid. This was then stirred at room temperature with 40 g of K2C03 in 80 mL of methanol for 18 h. The methanol was then removed in vacuo and the remains partitioned between DCM and sat. K2CO3 (aq). The combined organic extracts were passed through a hydrophobic frit and concentrated in vacuo to produce the title compound, 3.51 g., 123-90-0

The chemical industry reduces the impact on the environment during synthesis, 123-90-0, I believe this compound will play a more active role in future production and life.

Reference£º
Patent; ARROW THERAPEUTICS LIMITED; WO2005/89771; (2005); A1;,
Thiomorpholine – Wikipedia
Thiomorpholine | C4H9NS – PubChem

123-90-0, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route., 123-90-0

To a solution of thiomorpholine (1.0g, 9. 69MMOL) in acetic acid (11.5mL) cooled to 0¡ãC (ice bath) was added aqueous hydrogen peroxide solution (30percent w/v, 4mL) and the reaction heated to 100¡ãC for 16H. The mixture was cooled and solvent removed in vacuo before trituration of the residue with methanol gave a white precipitate. The solid was filtered and washed with methanol to give the title compound as an off-white powder. m/z (ES+) = 136. 06 [M+ H] +.

The chemical industry reduces the impact on the environment during synthesis, 123-90-0, I believe this compound will play a more active role in future production and life.

Reference£º
Patent; OSI PHARMACEUTICALS, INC.; WO2004/104001; (2004); A2;,
Thiomorpholine – Wikipedia
Thiomorpholine | C4H9NS – PubChem

123-90-0, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route., 123-90-0

To a solution of thiomorpholine (1.0g, 9. 69MMOL) in acetic acid (11.5mL) cooled to 0¡ãC (ice bath) was added aqueous hydrogen peroxide solution (30percent w/v, 4mL) and the reaction heated to 100¡ãC for 16H. The mixture was cooled and solvent removed in vacuo before trituration of the residue with methanol gave a white precipitate. The solid was filtered and washed with methanol to give the title compound as an off-white powder. m/z (ES+) = 136. 06 [M+ H] +.

The chemical industry reduces the impact on the environment during synthesis, 123-90-0, I believe this compound will play a more active role in future production and life.

Reference£º
Patent; OSI PHARMACEUTICALS, INC.; WO2004/104001; (2004); A2;,
Thiomorpholine – Wikipedia
Thiomorpholine | C4H9NS – PubChem

123-90-0, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route., 123-90-0

Example 11 Synthesis of 1-amino-3-(1,1-dioxo-lambda6-thiomorpholin-4-yl)-propan-2-ol To the solution of thiomorpholine (5.0 g, 48.7 mmol) in HOCH3 (200 mL) was added the solution of oxone (36.0 g, 58.5 mmol) in H2O (100 mL). The mixture was well stirred at 40¡ã C. for 48 h and then cooled to 0¡ã C. Aqueous NaOH was added dropwise to adjust pH=12. Solid was filtered out and washed with HOCH3 (3*40 mL). The combined liquid was condensed and purified by flash chromatograph on silica gel (CHCl3/CH30H/NH3.H2O=3/1/0.1-2/1/0.1) to give thiomorpholine 1,1-dioxide (6.2 g)in 93percent yield. 1H NMR (DMSO-d6) delta 2.97 (m, 4H), 3.07 (m, 4H), 3.42 (brs, 1H), MS (m/z) 136 (M+1)., 123-90-0

The chemical industry reduces the impact on the environment during synthesis, 123-90-0, I believe this compound will play a more active role in future production and life.

Reference£º
Patent; SUGEN, INC.; US2003/92917; (2003); A1;,
Thiomorpholine – Wikipedia
Thiomorpholine | C4H9NS – PubChem

123-90-0, A common heterocyclic compound, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route., 123-90-0

Example 11 Synthesis of 1-amino-3-(1,1-dioxo-lambda6-thiomorpholin-4-yl)-propan-2-ol To the solution of thiomorpholine (5.0 g, 48.7 mmol) in HOCH3 (200 mL) was added the solution of oxone (36.0 g, 58.5 mmol) in H2O (100 mL). The mixture was well stirred at 40¡ã C. for 48 h and then cooled to 0¡ã C. Aqueous NaOH was added dropwise to adjust pH=12. Solid was filtered out and washed with HOCH3 (3*40 mL). The combined liquid was condensed and purified by flash chromatograph on silica gel (CHCl3/CH30H/NH3.H2O=3/1/0.1-2/1/0.1) to give thiomorpholine 1,1-dioxide (6.2 g)in 93percent yield. 1H NMR (DMSO-d6) delta 2.97 (m, 4H), 3.07 (m, 4H), 3.42 (brs, 1H), MS (m/z) 136 (M+1).

The chemical industry reduces the impact on the environment during synthesis, 123-90-0, I believe this compound will play a more active role in future production and life.

Reference£º
Patent; SUGEN, INC.; US2003/92917; (2003); A1;,
Thiomorpholine – Wikipedia
Thiomorpholine | C4H9NS – PubChem

123-90-0, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. Thiomorpholine, cas is 123-90-0,the Thiomorpholine compound, it is a common compound, a new synthetic route is introduced below.

To a solution of thiomorpholine (1.0g, 9. 69MMOL) in acetic acid (11.5mL) cooled to 0¡ãC (ice bath) was added aqueous hydrogen peroxide solution (30percent w/v, 4mL) and the reaction heated to 100¡ãC for 16H. The mixture was cooled and solvent removed in vacuo before trituration of the residue with methanol gave a white precipitate. The solid was filtered and washed with methanol to give the title compound as an off-white powder. m/z (ES+) = 136. 06 [M+ H] +.

The chemical industry reduces the impact on the environment during synthesis,123-90-0,Thiomorpholine,I believe this compound will play a more active role in future production and life.

Reference£º
Patent; OSI PHARMACEUTICALS, INC.; WO2004/104001; (2004); A2;,
Thiomorpholine – Wikipedia
Thiomorpholine | C4H9NS – PubChem

123-90-0, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. Thiomorpholine, cas is 123-90-0,the Thiomorpholine compound, it is a common compound, a new synthetic route is introduced below.

Example 11 Synthesis of 1-amino-3-(1,1-dioxo-lambda6-thiomorpholin-4-yl)-propan-2-ol To the solution of thiomorpholine (5.0 g, 48.7 mmol) in HOCH3 (200 mL) was added the solution of oxone (36.0 g, 58.5 mmol) in H2O (100 mL). The mixture was well stirred at 40¡ã C. for 48 h and then cooled to 0¡ã C. Aqueous NaOH was added dropwise to adjust pH=12. Solid was filtered out and washed with HOCH3 (3*40 mL). The combined liquid was condensed and purified by flash chromatograph on silica gel (CHCl3/CH30H/NH3.H2O=3/1/0.1-2/1/0.1) to give thiomorpholine 1,1-dioxide (6.2 g)in 93percent yield. 1H NMR (DMSO-d6) delta 2.97 (m, 4H), 3.07 (m, 4H), 3.42 (brs, 1H), MS (m/z) 136 (M+1).

The chemical industry reduces the impact on the environment during synthesis,123-90-0,Thiomorpholine,I believe this compound will play a more active role in future production and life.

Reference£º
Patent; SUGEN, INC.; US2003/92917; (2003); A1;,
Thiomorpholine – Wikipedia
Thiomorpholine | C4H9NS – PubChem

123-90-0, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. Thiomorpholine, cas is 123-90-0,the Thiomorpholine compound, it is a common compound, a new synthetic route is introduced below.

9.98 g of thiomorpholine and 14.8 g of triflic anhydride were stirred together in DCM at room temperature for 2 hours. The reaction was then partitioned between 1 M K2C03 (aq) and DCM. The organic layer was separated and dried by passing through a hydrophobic frit, then concentrated in vacuo. 13.82 g of the resultant oil was stirred with 85.2 g of oxone in 50 mL of methanol and 50 mL of water for 18 h at room temperature. The reaction was then filtered and washed with methanol and the filtrate concentrated. This was then partitioned between water and EtOAc and the aqueous layer washed 3 times with EtOAc. The combined organic extracts were then dried (MgS04) and concentrated to produce a white solid. This was then stirred at room temperature with 40 g of K2C03 in 80 mL of methanol for 18 h. The methanol was then removed in vacuo and the remains partitioned between DCM and sat. K2CO3 (aq). The combined organic extracts were passed through a hydrophobic frit and concentrated in vacuo to produce the title compound, 3.51 g.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of Thiomorpholine, 123-90-0

Reference£º
Patent; ARROW THERAPEUTICS LIMITED; WO2005/89771; (2005); A1;,
Thiomorpholine – Wikipedia
Thiomorpholine | C4H9NS – PubChem