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
PROCEDURE
实验过程
TFA (10 mL) was added to a solution of tert-butyl 3-(2-chloro-3-((4-(2-ethylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)methyl)phenethoxy)propanoate [Example 26, step d] (3.1 g) in DCM (30 mL) and the resulting mixture stirred for 2 h, then evaporated. The residue was partitioned between ethyl acetate (100 mL) and saturated sodium bicarbonate solution (50 mL). The phases were separated and the aqueous phase was washed with more ethyl acetate (2×100 mL). The aqueous phase was then acidified with acetic acid and extracted with ethyl acetate (3×100 mL). The combined organic solutions were dried over sodium sulphate, filtered and evaporated to give the subtitled compound as a white foam. Yield 2.7 g.
WORKUP
后处理
- customevaporated
- customThe residue was partitioned between ethyl acetate (100 mL) and saturated sodium bicarbonate solution (50 mL)
- customThe phases were separated
- washthe aqueous phase was washed with more ethyl acetate (2×100 mL)
- extractionextracted with ethyl acetate (3×100 mL)
- dry with materialThe combined organic solutions were dried over sodium sulphate
- filtrationfiltered
- customevaporated