HRID1392420

反应详情

EQUATION

反应方程式

HRID 1392420 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The mixture of 4-[N-[1-[N-(furan-2-ylcarbonyl)amino]cyclohexanecarbonyl]amino]-1-(4-fluoro-2-aminophenyl)piperidin-3-ol (3.0 g) obtained in Step 2 of Example 87 and 2,5-dimethoxytetrahydrofuran (0.96 ml) was refluxed in 80 ml of acetic acid for 1 hour. The reaction mixture was concentrated under reduced pressure. The resulting residue was diluted with 70 ml of dichloromethane and washed with a saturated sodium bicarbonate and brine. The resulting organic layer was dried and concentrated on sodium sulfate. The resulting residue was purified with column chromatography to give 1.8 g of the titled compound as white color.

WORKUP

后处理

  1. concentrationThe reaction mixture was concentrated under reduced pressure
  2. additionThe resulting residue was diluted with 70 ml of dichloromethane
  3. washwashed with a saturated sodium bicarbonate and brine
  4. customThe resulting organic layer was dried
  5. concentrationconcentrated on sodium sulfate
  6. customThe resulting residue was purified with column chromatography