反応 #2227

ord-41e667fc94ef4b21b0e687948a96209d

反応方程式

O=Cc1ccc(Cl)cc1
4-chlorobenzaldehyde
CC(=O)CCC(=O)O
levulenic acid
C1CCNCC1
piperidine
Cc1ccccc1
toluene
O=C(O)CCC(=O)C=Cc1ccc(Cl)cc1
product
収率 44.0%
O=C(O)CCC(=O)C=Cc1ccc(Cl)cc1
3-(4-chlorocinnamoyl)-propionic acid
収率 44.0%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他To a dry 250 ml flask equipped with a magnetic stirrer
  2. 2
    温度Dean-Stark trap, and reflux condenser
  3. 3
    温度The reaction was refluxed for 3 hours
  4. 4
    温度The reaction was cooled
  5. 5
    その他to yield a reddish-brown liquid which
  6. 6
    その他was triturated with hexane

実験手順

To a dry 250 ml flask equipped with a magnetic stirrer, Dean-Stark trap, and reflux condenser was charged 15 g of 4-chlorobenzaldehyde, 12.4 g levulenic acid, 5.7 ml of piperidine, and 100 ml of toluene. The reaction was refluxed for 3 hours, after which no water was observed to azeotrope from the solution. The reaction was cooled and stripped to yield a reddish-brown liquid which was triturated with hexane to yield 11.2 g of product as a yellow solid.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US05728698uspto-grants-1998_03