HRID601624

反应详情

EQUATION

反应方程式

HRID 601624 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

N-Hydroxy-butyramidine (0.425 g, 4.16 mmol) in DMF (2 ml) is added to a stirred suspension of sodium hydride (0.183 g of a 60% dispersion in oil, 4.58 mmol) in the presence of molecular sieves (0.4 g). The reaction flask is then immersed in a pre-heated oil bath at 50° C. and stirring continued for 5 min. 3-tert-Butoxycarbonylamino-propionic acid ethyl ester (0.904 g, 4.16 mmol) in DMF (2 ml) is added over 5 min followed by more DMF (2 ml). After 3 h at 50° C. the mixture is cooled to 0° C. and water (3 ml) is added. The mixture is allowed to warm to room temperature then filtered through Celite™ filter material, washing with ethyl acetate, and the solvent is removed. Purification by chromatography, eluting with DCM:MeOH (95:5 increasing to 85:15) affords the titled compound.

WORKUP

后处理

  1. customThe reaction flask is then immersed in a pre-heated oil bath at 50° C.
  2. temperatureto warm to room temperature
  3. filtrationthen filtered through Celite™
  4. filtrationfilter material
  5. washwashing with ethyl acetate
  6. customthe solvent is removed
  7. customPurification by chromatography
  8. washeluting with DCM:MeOH (95:5 increasing to 85:15)