反応 #2028887

ord-9b9dc4fd40474022806e97056924a4ff

反応方程式

Cl
hydrochloric acid
CCOC=O
Ethyl formate
CC(=O)c1ccc(Cl)cc1
4′-chloroacetophenone
C[O-].[Na+]
Sodium methoxide
O=CCC(=O)c1ccc(Cl)cc1
yellow oil
収率 100.2%
O=CCC(=O)c1ccc(Cl)cc1
3-[4-(chloro)phenyl]-propane-1,3-dione
収率 100.2%

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The phases were separated
  2. 2
    洗浄the ethereal solution washed with brine
  3. 3
    乾燥dried over magnesium sulfate
  4. 4
    ろ過filtered
  5. 5
    濃縮concentrated in vacuo

実験手順

Ethyl formate (8.15 g, 0.11 mol) and 4′-chloroacetophenone (15.4 g, 0.1 mol) were stirred in ether (150 mL) at room temperature. Sodium methoxide (25%) (23.77 g, 0.11 mol) was added dropwise. The mixture was stirred at room temperature for 16 hours and was then treated with 150 mL of 1N hydrochloric acid. The phases were separated and the ethereal solution washed with brine, dried over magnesium sulfate, filtered and concentrated in vacuo to afford 18.3 g of a yellow oil. The resulting crude mixture was used directly in the next step without purification.

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: USRE044048E1uspto-grants-2013_03