HRID1455365

反应详情

EQUATION

反应方程式

HRID 1455365 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

Preparation H7, Step 1: To a soultion of 3-(methoxycarbonyl)benzoic acid (800 mg, 4.4 mmol) in DMF (15 mL) at rt was added HATU (2g, 5.3 mmol), 3-aminopropanenitrile (0.33 mL, 4.4 mmol), and iPr2NEt (0.92 mL, 5.3 mmol). The mixture was stirred at rt for 16 h before water and EtOAc were added. The organic layer was separated and re-washed twice before it was collected, dried over Na2SO4, and concentrated to provide methyl 3-((2-cyanoethyl)carbamoyl)benzoate as a glassy solid (900 mg). MS found: (M+H)+=233.

WORKUP

后处理

  1. customPreparation H7, Step 1
  2. additionwere added
  3. customThe organic layer was separated
  4. washre-washed twice before it
  5. customwas collected
  6. dry with materialdried over Na2SO4
  7. concentrationconcentrated