With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.76176-87-9,Thiomorpholine-1-oxide hydrochloride,as a common compound, the synthetic route is as follows.,76176-87-9
To a solution of 6-chloro-3-pyridazinecarboxaldehyde (1) (502 mg, 3.52 mmol, 1.0 eq) in 1 ,2-dichloroethane (4 ml_) was added NaOAc (722 mg, 8.80 mmol, 2.5 eq) followed by CH2CI2 (2 ml_) and thiomorpholine-1 -oxide hydrochloride (2) (1.37 g, 8.80 mmol, 2.5 eq). The mixture was stirred for 10 min before the addition of NaBH(OAc)3 (1.12 g, 5.28 mmol, 1.5 eq) then stirred for 4 h at room temperature. The reaction was quenched with 1 M NaOH (5 ml_) and the resulting mixture was poured into H20 (10 ml_) and extracted with CH2CI2 (10 ml_) then EtOAc (2 x 10 ml_). The combined organic extracts were dried over MgS04, filtered and concentrated in vacuo. Purification by silica gel chromatography using CH2CI2/MeOH (1 :0-19: 1 ) yielded intermediate 3 as an off- white solid (408 mg, 47%). (1335) LCMS (ES): Found 245.9 [M+Hf. (1336) 1H NMR (300MHz, DMSO-cf6), d: 7.91 (d, J=8.9 Hz, 1 H), 7.81 (d, J=8.9 Hz, 1 H), 3.89 (s, 2H), 2.82-3.04 (m, 4H), 2.59-2.79 (m, 4H).
The synthetic route of 76176-87-9 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; KARUS THERAPEUTICS LIMITED; SHUTTLEWORTH, Stephen Joseph; GATLAND, Alice Elizabeth; FINNEMORE, Daniel John; ALEXANDER, Rikki Peter; SILVA, Franck; CECIL, Alexander; (233 pag.)WO2019/166824; (2019); A1;,
Thiomorpholine – Wikipedia
Thiomorpholine | C4H9NS – PubChem