HRID1180800
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
To a stirred solution at room temperature of VI (745 mg, 2.84 mmol) in CH2Cl2 (10 ml) was added trifluoroacetc acid (6 ml, 95% in water). After 27 h, the reaction mixture was concentrated, and triturated in water. After 1 h, the suspension was filtered off, rinsed with H2O, and dried to afford the title compound VII (556 mg, 2.70 mmol, 95% yield) as an off-white solid. 1H NMR (300 MHz, DMSO-d6) δ(ppm): AB system (δA=8.01, δB=7.88, J=8.1 Hz, 4H), 7.68 (d, J=15.8 Hz, 1H), 6.70 (d, J=16.3 Hz, 1H), 3.90 (s, 3H).
WORKUP
后处理
- concentrationthe reaction mixture was concentrated
- customtriturated in water
- waitAfter 1 h
- filtrationthe suspension was filtered off
- washrinsed with H2O
- customdried