HRID1354238
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
- 100 °C
PROCEDURE
实验过程
Sodium methoxide in methanol (25 w/w %, 0.5 ml) is added to a solution of compound 45 (50 mg, 0.124 mmol) in NMP (0.5 ml). The resulting mixture is heated to 100° C. overnight, then cooled to room temperature, diluted with 50% EtOAc in hexane, washed with water, brine, dried, filtered and evaporated. The crude product is purified by chromatography (eluted with 6% EtOAc in hexane) to give the product as colorless oil. 1H NMR (CDCl3) δ 1.00 (t, J=7.6 Hz, 6H), 1.75 (m, 4H), 2.04 (s, 3H), 3.80 (s, 3H), 3.94 (s, 3H), 4.12 (m. 1H), 6.78 (s, 1H), 6.89 (dd, 1H), 6.92 (s, 1H), 7.30 (d, J=8.4 Hz, 1H). LCMS 400.4 (M+1).
WORKUP
后处理
- temperaturecooled to room temperature
- washwashed with water, brine
- customdried
- filtrationfiltered
- customevaporated
- customThe crude product is purified by chromatography (eluted with 6% EtOAc in hexane)