反応 #10481

ord-1a5375979fb5402d8fe980b291f4b317

反応方程式

Cc1ccc(C2(C(=O)O)CC2C(=O)O)cc1
1-(4-methylphenyl)-1,2-cyclopropanedicarboxylic acid
NC(N)=O
urea
Cc1ccc(C23CC2C(=O)NC3=O)cc1
(±)-1-(4-methylphenyl)-3-azabicyclo[3.1.0]hexan-2,4-dione

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    温度was heated
  2. 2
    温度to reflux
  3. 3
    温度at reflux until the reaction
  4. 4
    その他On completion of the reaction period
  5. 5
    温度the solution was cooled to 80–90° C.
  6. 6
    洗浄washed with water (69 L)

実験手順

A mixture of purified 1-(4-methylphenyl)-1,2-cyclopropanedicarboxylic acid (58 kg), toluene (465 kg) and urea (23.8 kg) was heated to reflux and the mixture held at reflux until the reaction was complete. On completion of the reaction period, the solution was cooled to 80–90° C. and washed with water (69 L). The lower aqueous layer was discarded. In this way (±)-1-(4-methylphenyl)-3-azabicyclo[3.1.0]hexan-2,4-dione was obtained as a solution in toluene.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US07094799B2uspto-grants-2006_08