HRID1527375

反应详情

EQUATION

反应方程式

HRID 1527375 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of (2S,4S)-4-(9H-fluoren-9-ylmethoxycarbonylamino)-pyrrolidine-2-carboxylic acid benzyl ester (3.03 g, 5.45 mmol) and Et3N (1.1 mL, 8.2 mmol) in dry THF (60 mL) was added a solution of 3-isocyanato-indole-1-carboxylic acid amide (1.1 g, 5.4 mmol, prepared as described in Scheme A1) in dry THF (60 mL). The resulting solution was stirred at RT under nitrogen for 20 min. The mixture was poured into water and extracted twice with EtOAc. The combined organic layers were dried over Na2SO4, filtered and concentrated under high vacuum (the temperature of the water bath of the rotary evaporator was kept to RT) to give the title compound. Rf (c-hexane/EtOAc 1:3)=0.39; MS (LCMS): 644.2 [M+H]+, 666.2 [M+Na]+; tR (HPLC conditions a): 4.0 min.

WORKUP

后处理

  1. extractionextracted twice with EtOAc
  2. dry with materialThe combined organic layers were dried over Na2SO4
  3. filtrationfiltered
  4. concentrationconcentrated under high vacuum (
  5. customthe temperature of the water bath of the rotary evaporator
  6. customwas kept to RT