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
- 85 °C
PROCEDURE
实验过程
tert-Butyl 5-(benzyloxy)-6-hydroxy-2-(2-methyl-2-phenylpropyl)pyrimidine-4-carboxylate (55) (260 mg, 598 μmol, Eq: 1.00) was stirred in tetrahydrofuran/water. Lithium hydroxide monohydrate (126 mg, 2.99 mmol, Eq: 5) was added. The reaction mixture was heated at 85° C. for 7 hours, cooled, and stirred at room temperature for 16 hours. 1N HCl was added until precipitate forms (about 10 ml). The mixture was diluted with water, extracted three times with ethyl acetate, washed with brine and dried over magnesium sulfate. The solvent was removed on a rotary evaporator to give 5-(benzyloxy)-6-hydroxy-2-(2-methyl-2-phenylpropyl)pyrimidine-4-carboxylic acid (56) as a white solid (155 mg, 68%).
WORKUP
后处理
- temperaturecooled
- extractionextracted three times with ethyl acetate
- washwashed with brine
- dry with materialdried over magnesium sulfate
- customThe solvent was removed on a rotary evaporator