反应 #9723

ord-ac4f6997785540cfabd1e40607d0df66

反应方程式

O=C(OO)c1cccc(Cl)c1
m-chloroperbenzoic acid
[I-].[K+]
potassium iodide
CCOC(=O)C(C)(C)Oc1ccc(C(C)=O)cc1C
ethyl 2-(4-acetyl-2-methylphenoxy)-2-methylpropanoate
CCOC(=O)C(C)(C)Oc1ccc(C(C)=O)cc1C
intermediate 8
CCOC(=O)C(C)(C)Oc1ccc(C(C)=O)cc1C
ethyl 2-(4-acetyl-2-methylphenoxy)-2-methylpropanoate
Cc1ccc(S(=O)(=O)O)cc1
4-toluenesulphonic acid
CCOC(=O)C(C)(C)Oc1ccc(OC(C)=O)cc1C
title compound
CCOC(=O)C(C)(C)Oc1ccc(OC(C)=O)cc1C
ethyl 2-[4-(acetyloxy)-2-methylphenoxy]-2-methylpropanoate

反应条件

温度
40°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The organic layer was collected
  2. 2
    洗涤washed twice with water and brine
  3. 3
    干燥dried over sodium sulfate
  4. 4
    过滤filtered
  5. 5
    浓缩the filtrate concentrated

实验过程

A solution of ethyl 2-(4-acetyl-2-methylphenoxy)-2-methylpropanoate (intermediate 8, 37.33 g) in dichloromethane (650 ml) was treated with 4-toluenesulphonic acid (2.75 g) followed by m-chloroperbenzoic acid (60.5 g) and the mixture warmed to 40° C. and stirred under nitrogen for 19 hours. The cooled mixture was treated with dichloromethane (350 ml) and the resulting mixture added to aqueous potassium iodide (1000 ml, 10% solution). The organic layer was collected and washed twice with water and brine, then dried over sodium sulfate, filtered and the filtrate concentrated to give the title compound as an orange oil.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07091237B2uspto-grants-2006_08