HRID604242

反应详情

EQUATION

反应方程式

HRID 604242 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Boc-Val-OH (2.00 g.,9.26 mmol) and DCC (1.90 g, 9.26 mmol) were dissolved in dry DMF (20 ml) under a nitrogen atmosphere. The mixture was stirred continuously for one hour at 0° C. A solution of quinidine (1.50 g, 4.63 mmol) and DMAP (0.06 g, -0.65 mmol) in DMF (100 ml) was added dropwise to the reaction mixture at 0° C. The reaction mixture was stirred and allowed to warm to room temperature. After 24 hours, the reaction was checked by TLC (1:13 methanol/dichloromethane mixture) and LC-MS analysis, and was found to be complete. The urea derivative was removed by filtration and washed with ethyl acetate. Solvents from the combined filtrate and washing were totally removed under reduced pressure.

WORKUP

后处理

  1. stirringThe reaction mixture was stirred
  2. temperatureto warm to room temperature
  3. waitAfter 24 hours
  4. customThe urea derivative was removed by filtration
  5. washwashed with ethyl acetate
  6. washSolvents from the combined filtrate and washing
  7. customwere totally removed under reduced pressure