HRID5522
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 solution of 1-methyl-4-(3,4-diacetoxybenzoyl)piperazine (295 mg) n methanol (3 ml) was added a saturated potassium carbonate solution is methanol (6 ml) and the mixture was stirred at room temperature for 30 minutes. The mixture was poured into ice water and adjusted to pH 9 with 1N hydrochloric acid. The mixture was extracted several times with a mixture of chloroform and methanol (20:1 V/V) and the organic layer was washed with brine, dried over magnesium sulfate and evaporated in vacuo. The residue was crystallized by addition of ethyl acetate to give 1-methyl-4-(3,4-dihydroxybenzoyl)piperazine (71 mg) as white crystal.
WORKUP
后处理
- extractionThe mixture was extracted several times
- additionwith a mixture of chloroform and methanol (20:1 V/V)
- washthe organic layer was washed with brine
- dry with materialdried over magnesium sulfate
- customevaporated in vacuo
- customThe residue was crystallized by addition of ethyl acetate