反応 #302857

ord-0fda36c95d0a4a968ebfdb678629eeee

反応方程式

COc1ccc(O)c(C(C)=O)c1
5′-methoxy-2′-hydroxyacetophenone
O=C(Cl)c1ccc([N+](=O)[O-])cc1
4-nitrobenzoyl chloride
Cl
hydrochloric acid
COc1ccc(OC(=O)c2ccc([N+](=O)[O-])cc2)c(C(C)=O)c1
compound 21
COc1ccc(OC(=O)c2ccc([N+](=O)[O-])cc2)c(C(C)=O)c1
4-nitrobenzoic acid 2-acetyl-4-methoxyphenyl ester

溶媒

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

  1. 1
    その他The obtained mixture was reacted at room temperature for 30 minutes
  2. 2
    温度under cooling on ice
  3. 3
    ろ過The obtained precipitate was collected by filtration
  4. 4
    洗浄the filtrate was then washed with purified water

実験手順

5′-methoxy-2′-hydroxyacetophenone (1.5 g, 9.03 mmol) was added to a pyridine solution (20 ml) that contained 4-nitrobenzoyl chloride (1.72 g, 9.26 mmol) in an ice bath. The obtained mixture was reacted at room temperature for 30 minutes, and the reaction solution was then poured into 1 N hydrochloric acid under cooling on ice. The obtained mixture was intensively stirred. The obtained precipitate was collected by filtration, and the filtrate was then washed with purified water, so as to obtain a product of interest, 4-nitrobenzoic acid 2-acetyl-4-methoxyphenyl ester (compound 21). Yield: 2.49 g (yield constant: 87.4%)

出典

DOI: 10.6084/m9.figshare.5104873.v1特許: US08192717B2uspto-grants-2012_06