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
3-{[4-(Azetidin-1-ylcarbonyl)-2-chlorophenyl]oxy}-5-{[(1S)-2-hydroxy-1-methylethyl]oxy}-N-(1-methyl-1H-pyrazol-3-yl)benzamide (104 mg, 0.215 mmol) was dissolved in methanol (3 mL) and THF (3 mL). Triethylamine (65 mg, 0.644 mmol) was added and the flask evacuated and purged with nitrogen (3 times). 10% Palladium on carbon (25 mg) was added and the flask further evacuated and finally purged with hydrogen gas. The reaction mixture was stirred at ambient temperature for 16 hours until completion. The reaction mixture was evacuated and purged with nitrogen (3 times). The catalyst was filtered off, the filtrate concentrated in vacuo and dissolved in ethyl acetate (10 mL), washed with water (2×10 mL, saturated aqueous sodium chloride solution (10 mL) and dried (MgSO4) to give the title compound (95 mg).
WORKUP
后处理
- customthe flask evacuated
- custompurged with nitrogen (3 times)
- addition10% Palladium on carbon (25 mg) was added
- customthe flask further evacuated
- customfinally purged with hydrogen gas
- customThe reaction mixture was evacuated
- custompurged with nitrogen (3 times)
- filtrationThe catalyst was filtered off
- concentrationthe filtrate concentrated in vacuo
- dissolutiondissolved in ethyl acetate (10 mL)
- washwashed with water (2×10 mL, saturated aqueous sodium chloride solution (10 mL)
- dry with materialdried (MgSO4)