反応 #169391

ord-31cc3862d3244285a6a75e5c3f5b4c7c

反応方程式

CCOC(=O)CC(=O)CCl
Ethyl 4-chloroacetoacetate
NC(=O)C1CC1
cyclopropanecarboxamide
CCOC(=O)Cc1coc(C2CC2)n1
title compound
収率 50.0%
CCOC(=O)Cc1coc(C2CC2)n1
Ethyl (2-cyclopropyl-1,3-oxazol-4-yl)acetate
収率 50.0%

反応条件

温度
120°CELSIUS
詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他then evaporated in vacuo
  2. 2
    その他The crude solid was purified by column chromatography on silica gel (80:20 petroleum ether: EtOAc)

実験手順

Ethyl 4-chloroacetoacetate (20.0 g, 122.0 mmol) was added to cyclopropanecarboxamide (3.52 g, 41.5 mmol) in toluene (100 mL) and 1,4-dioxane (100 mL). The mixture was refluxed at 120° C. for 17 hours then evaporated in vacuo. The crude solid was purified by column chromatography on silica gel (80:20 petroleum ether: EtOAc) to afford the title compound as a white solid in 50% yield, 4.00 g.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08846698B2uspto-grants-2014_09