HRID1088698
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
To a solution of the product of Example 14 (1.5 g) in pyridine (10 mL) at 0° C. was added dropwise dimethyl carbamyl chloride (0.52 mL) and the resulting solution was heated at 70°-80° C. for 24 hours. The pyridine was removed and the reaction diluted with CH2Cl2, washed with water (3x), brine, dried (MgSO4), filtered and concentrated. Chromatography of the residue on silica gel (elution with 1% CH2OH/CH2Cl2) provided 1.29 g of the desired product.
WORKUP
后处理
- temperaturethe resulting solution was heated at 70°-80° C. for 24 hours
- customThe pyridine was removed
- additionthe reaction diluted with CH2Cl2
- washwashed with water (3x), brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated