HRID30169

反应详情

EQUATION

反应方程式

HRID 30169 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2-Carboxymethyl-piperidine-1-carboxylic acid tert butyl ester (2.0 g) was added to [O-(7-azabenzotriazol-1-yl)-1,1,3,3-tetramethyluronium hexafluorophosphate] (3.13 g) in dimethylformamide (10 ml) containing diisopropylethylamine (3.2 g) and the mixture stirred for 15 min. 2-Furoic acid hydrazide (1.04 g) was then added and stirring continued for 16 h. The reaction mixture was diluted with water and extracted with diethyl ether. The combined ether extracts were washed with water, dried and solvent removed at reduced pressure the residue was column chromatographed (silica gel, 20-50% ethyl acetate/hexane) to give the title compound (2.05 g).

WORKUP

后处理

  1. stirringstirring
  2. waitcontinued for 16 h
  3. extractionextracted with diethyl ether
  4. washThe combined ether extracts were washed with water
  5. customdried
  6. customsolvent removed at reduced pressure the residue
  7. customchromatographed (silica gel, 20-50% ethyl acetate/hexane)