HRID548676
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 50 °C
PROCEDURE
实验过程
10% Palladium on carbon (30 mg) was added to 3-{[1,1-dioxido-2-(phenylmethyl)-3,4-dihydro-2H-5,1,2-benzoxathiazepin-7-yl]oxy}-5-{[(1S)-2-hydroxy-1-methylethyl]oxy}-N-(1-methyl-1H-pyrazol-3-yl)benzamide (100 mg; 0.17 mmol) in dry THF (4 mL) and dry ethanol (4 mL) under an argon atmosphere. The reaction was degassed and placed under a hydrogen atmosphere then stirred for 24 hours at 50° C. and 20 bar. The mixture was filtered through diatomaceous earth and the filtrate evaporated. Purification via column chromatography, eluting with 50-100% ethyl acetate in isohexane, yielded a colourless oil which solidified under vacuum to give the title compound as a white foam (21 mg).
WORKUP
后处理
- customThe reaction was degassed
- filtrationThe mixture was filtered through diatomaceous earth
- customthe filtrate evaporated
- customPurification via column chromatography
- washeluting with 50-100% ethyl acetate in isohexane
- customyielded a colourless oil which