反应详情

温度

20 °C

To a solution of 4-[5-(bromomethyl)-1,3-oxazol-2-yl]-6-chloro-1-(phenylsulfonyl)-1H-indazole (750 mg, 1.657 mmol) in dichloromethane (50 mL) stirred in air at room temp, was added neat 2,6-dimethylmorpholine (191 mg, 1.657 mmol, available from Aldrich as a mixture of isomers). The reaction mixture was stirred at 20° C. for 20 hr. Volatiles were removed using a rotary evaporator then the crude material was pre-absorbed onto Fluorosil™ and purified by column chromatography on silica (100 g) using a 0-100% ethyl acetate-cyclohexane gradient over 60 mins. Two diastereoisomers were isolated. Appropriate fractions were combined and evaporated in vacuo to give the title compound as a yellow oil (226 mg).

1. additionavailable from Aldrich as a mixture of isomers)
2. customVolatiles were removed
3. customa rotary evaporator
4. customthe crude material was pre-absorbed onto Fluorosil™
5. custompurified by column chromatography on silica (100 g)
6. customover 60 mins
7. customTwo diastereoisomers were isolated
8. customevaporated in vacuo