HRID2121862
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
An ice-cooled solution of the product from Step B (298 g, 0.95 mol) in THF (3 L) was treated with 1 M aqueous sodium hydroxide (1.95 L, 1.9 mol) keeping the temperature below 8° C. After the starting material was consumed, the mixture was diluted with brine and extracted twice with ethyl ether. The organic solution was washed with water until neutral and then with brine, dried over sodium sulfate, treated with charcoal and passed through silica (1 kg) with ether and with 1:1 ethyl acetate-hexane to yield, after concentration in vacuo, a yellow solid (207 g, 76%).
WORKUP
后处理
- customthe temperature below 8° C
- customAfter the starting material was consumed
- additionthe mixture was diluted with brine
- extractionextracted twice with ethyl ether
- washThe organic solution was washed with water until neutral and then with brine
- dry with materialdried over sodium sulfate
- additiontreated with charcoal
- customto yield
- concentrationafter concentration in vacuo