HRID1949630

反应详情

EQUATION

反应方程式

HRID 1949630 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

To a solution containing Cbz-N(Me)Ala-OH (119 mg, 0.5 mmol) in anhydrous NMP (4 mL) was cooled to 0° C. HATU (189 mg, 0.5 mmol) and DIPEA (111 mg, 0.8 mmol) were added followed by the addition of crude 44 (280 mg, 0.5 mmol) in anhydrous NMP (4 mL). The reaction mixture was slowly warmed to ambient temperature. After 2 h, the reaction mixture was diluted with EtOAc and washed successively with 1M HCl, aqueous NaHCO3, and brine, dried over anhydrous Na2SO4, filtered, and concentrated to afford 330 mg of crude 45 as an amber-colored oil which was used without further purification. Mass spectrum, m/z [756.4] (M+H)+.

WORKUP

后处理

  1. temperatureThe reaction mixture was slowly warmed to ambient temperature
  2. washwashed successively with 1M HCl, aqueous NaHCO3, and brine
  3. dry with materialdried over anhydrous Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated