反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
CONDITIONS
反应条件
- 温度
- 120 °C
PROCEDURE
实验过程
The reaction mixture of (S)-2-tert-butoxy-2-(7-(4-chlorophenyl)-2-(3-(2-chloropyridin-4-yl)phenyl)-5-methylbenzo[d]thiazol-6-yl)ethyl pivalate (16 mg, 0.025 mmol), 1-methylpiperazine (1 mL) was heated at 120° C. overnight. Then the reaction mixture was washed by sat. NaHCO3, extracted by EtOAc, the organic phase was dried over MgSO4, filtered, concentrated. To the residue was added THF, MeOH, 2N NaOH, the mixture was heated at 45° C. After the reaction finished, the reaction was washed by sat NaHCO3, extracted by EtOAc, the organic phase was dried over MgSO4, filtered, concentrated down and purified by silica gel column, eluting by 0-100% EtOAc in hexanes to give the product. LCMS-ESI+: calc'd for C36H39ClN4O2S: 627.2 (M+H+); Found: 627.3 (M+H+).
WORKUP
后处理
- washThen the reaction mixture was washed by sat. NaHCO3
- extractionextracted by EtOAc
- dry with materialthe organic phase was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- additionTo the residue was added THF, MeOH, 2N NaOH
- temperaturethe mixture was heated at 45° C
- washthe reaction was washed
- extractionextracted by EtOAc
- dry with materialthe organic phase was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated down
- custompurified by silica gel column
- washeluting by 0-100% EtOAc in hexanes
- customto give the product