HRID452461
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
PROCEDURE
实验过程
4-bromo-2,5-difluorobenzoic acid (4.82 g, 20.3 mmol) and methanol (100 ml, saturated with gaseous HCl) was heated at 65° C. for 3 h. The volatiles were evaporated, MeOH was added and once again it was evaporated. This procedure was repeated three times. Purification by flash column chromatography (isooctane/EtOAc 4:1) gave the title compound (4.2 g). MS m/z (rel. intensity, 70 eV) 252 (M+, 33), 250 (M+, 34), 221 (95), 219 (bp), 193 (20), 191 (21), 112 (32).
WORKUP
后处理
- customThe volatiles were evaporated
- additionMeOH was added
- customonce again it was evaporated
- customPurification by flash column chromatography (isooctane/EtOAc 4:1)