HRID1654587

反应详情

EQUATION

反应方程式

HRID 1654587 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Z-Tle (15.6 g, 59.1 mmol), Leu-OEt HCl (11.56 g, 59.1 mmol), and N-methyl morpholine (NMM) (12.75 mL) are mixed with 45 mL of DMF and a cloudy suspension forms. The mixture is cooled to 0° C. and treated with TBTU (19.1 g, 59.48 mmol), then stirred at 0° C. for 15 minutes, then removed from the cold bath and stirred for 1.5 hours. The mixture is poured into 500 mL of a saturated solution of sodium carbonate which is then extracted with two 350 mL portions of ethyl acetate. The combined organic extracts are washed with 500 mL of 1 M KHSO4 water and brine and then dried over sodium sulfate. The solvents are removed to give Z-Tle-Leu-OEt (24.1 g). FABMS M+1 407

WORKUP

后处理

  1. customremoved from the cold bath
  2. stirringstirred for 1.5 hours
  3. additionThe mixture is poured into 500 mL of a saturated solution of sodium carbonate which
  4. extractionis then extracted with two 350 mL portions of ethyl acetate
  5. washThe combined organic extracts are washed with 500 mL of 1 M KHSO4 water and brine
  6. dry with materialdried over sodium sulfate
  7. customThe solvents are removed