HRID531447
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
A stirred solution of 5-bromo-6-cyclopropyl-3-((trimethylsilyl)ethynyl)pyridin-2-amine (1 g, 3.2 mmol), tert-butanol (10 mL) was added potassium tert-butoxide (1.45 g, 12.9 mmol) and stirred at ambient temperature for 15 min. RM was quenched with water and extracted with ethyl acetate, organic portion was dried over sodium sulfate and concentrated to give 1.2 g of the titled compound. 1H NMR (CDCl3, 300 MHz): δ 7.86-7.85 (m, 1H), 6.45-6.42 (m, 1H), 4.98-4.96 (m, 1H), 4.88-4.7 (m, 1H), 4.55 (s, 2H), 2.35-2.31 (m, 1H), 2.0 (s, 9H), 1.04-0.86 (m, 4H). LCMS: m/z=311.1 (M+1).
WORKUP
后处理
- customRM was quenched with water
- extractionextracted with ethyl acetate, organic portion
- dry with materialwas dried over sodium sulfate
- concentrationconcentrated