HRID1182116
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
A solution of 5-Ethyl-2-methyl-2H-pyrazol-3-ylamine (10 g, 79.8 mmol) (500 ml) and potassium carbonate in THF (12.14 g, 87.8 mmol) is cooled to 0° C. Phenylchloroformate (10.15 ml, 80.6 mmol) is added dropwise over 20 minutes. The reaction mixture is stirred for 40 minutes at 0° C. then allowed to warm to ambient temperature and stirred for a further 2.5 hours. The reaction mixture is partitioned between ethylacetate and water. The organic phase is washed with 5% aqueous citric acid solution and brine. The organic phase is treated with MgSO4 and charcoal then filtered and evaporated to afford (5-Cyclopropyl-2-methyl-2H-pyrazol-3-yl)-carbamic acid phenyl ester. [M+H] 246.21
WORKUP
后处理
- temperatureto warm to ambient temperature
- stirringstirred for a further 2.5 hours
- customThe reaction mixture is partitioned between ethylacetate and water
- washThe organic phase is washed with 5% aqueous citric acid solution and brine
- additionThe organic phase is treated with MgSO4 and charcoal
- filtrationthen filtered
- customevaporated