HRID1088698

反应详情

EQUATION

反应方程式

HRID 1088698 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. temperaturethe resulting solution was heated at 70°-80° C. for 24 hours
  2. customThe pyridine was removed
  3. additionthe reaction diluted with CH2Cl2
  4. washwashed with water (3x), brine
  5. dry with materialdried (MgSO4)
  6. filtrationfiltered
  7. concentrationconcentrated