Dimethyl Sulfoxide → HCID 59334563、化合物

To a solution of oxalyl chloride (2.93 mL, 34.6 mmol) in 30 dichloromethane (50 mL) was added dimethyl sulfoxide (3.68 mL, 51.9 mmol) at −78° C. To the reaction mixture was added a solution of (7-chloro-2-methyl-2H-indazol-4-yl)methanol (3.40 g, 17.3 mmol) in dichloromethane (10 mL), and the mixture was stirred for 2 hr. To the reaction mixture was added triethylamine (14.6 mL, 104 mmol) at −78° C., and the mixture was stirred for 30 min. The reaction mixture was warmed to room temperature, and the mixture was stirred at room temperature for 4 hr. To the reaction mixture was added saturated aqueous ammonium chloride solution, and the aqueous layer was extracted with dichloromethane. The combined extract was washed with saturated brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The obtained crude product was purified by recrystallization (hexane/dichloromethane) to give the title compound (3.07 g, yield 91%).

1. stirringthe mixture was stirred for 30 min
2. stirringthe mixture was stirred at room temperature for 4 hr
3. extractionthe aqueous layer was extracted with dichloromethane
4. extractionThe combined extract
5. washwas washed with saturated brine
6. dry with materialdried over anhydrous sodium sulfate
7. customthe solvent was evaporated under reduced pressure
8. customThe obtained crude product
9. customwas purified by recrystallization (hexane/dichloromethane)

ORDレコード

ord-296404055eb24ca6af08244a7aab3257

出典データセット

uspto-grants-2012_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08110585B2