HRID1392416

反应详情

EQUATION

反应方程式

HRID 1392416 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The solution of 4-[N-[1-[N-(furan-2-ylcarbonyl)amino]cyclohexanecarbonyl]amino]-1-(4-fluoro-2-aminophenyl)piperidin-3-ol (1.0 g, 2.24 mmol) obtained in Step 2 in 30 ml of tetrahydrofuran was cooled to 0° C. Sodium carbonate (350 mg, 3.36 mmol) and methoxyacetyl chloride (0.53 mg, 5.82 mmol) was added to the reaction mixture, which was then stirred for 4 hours. 20 ml of ice water was added to the reaction mixture, which was then concentrated and extracted with 50 ml of ethyl acetate. The resulting organic layer was dried and concentrated on sodium sulfate. The resulting residue was crystallized with ethyl acetate to give 1.1 g of the titled compound.

WORKUP

后处理

  1. concentrationwas then concentrated
  2. extractionextracted with 50 ml of ethyl acetate
  3. customThe resulting organic layer was dried
  4. concentrationconcentrated on sodium sulfate
  5. customThe resulting residue was crystallized with ethyl acetate