HRID1042335
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
- 0 °C
PROCEDURE
实验过程
A solution of N-(6-bromopyridin-2-yl)-2,2-dimethylpropanamide (2 g, 7.77 mmol, 1 eq.) in 25 ml of THF was cooled to −78° C. and n-BuLi (1.6 M, 9.72 ml, 15.55 mmol) was added dropwise. After 1 h, acetaldehyde (0.376 g, 8.55 mmol, 1.1 eq.) was added and the mixture was warmed to 0° C. within 1 h. The reaction was quenched with H2O, and diluted with EtOAc. The aqueous layer was separated and extracted with EtOAc. The organics were combined, dried over MgSO4 and concentrated. The crude material was purified by chromatography on silica gel to give N-[6-(1-hydroxyethyl)pyridin-2-yl]-2,2-dimethylpropanamide (1.45 g, 83% yield) as a white solid.
WORKUP
后处理
- customThe reaction was quenched with H2O
- additiondiluted with EtOAc
- customThe aqueous layer was separated
- extractionextracted with EtOAc
- dry with materialdried over MgSO4
- concentrationconcentrated
- customThe crude material was purified by chromatography on silica gel