反应 #1810822

反应方程式

2-chloro-5-methanesulfonyl-benzoic acid

2,2,2-trifluoro-ethanol

→

title compound

5-methanesulfonyl-2-(2,2,2-trifluoro-ethoxy)-benzoic acid

溶剂

NEt3

反应条件

后处理

1. 1
   其他The volatiles were removed under vacuum
2. 2
   萃取Extraction with ethyl acetate
3. 3
   其他drying of the combined organic fractions and evaporation
4. 4
   其他yielded a residue which
5. 5
   其他was purified by reversed phase preparative HPLC
6. 6
   洗涤eluting with an acetonitrile/water gradient
7. 7
   其他Evaporation of the product fractions

实验过程

A mixture of 2.13 mmol 2-chloro-5-methanesulfonyl-benzoic acid, 0.64 mmol Cu(I)Br in 5 ml NEt3 and 25 ml 2,2,2-trifluoro-ethanol was heated to 120° C. for 16 h in a sealed tube. The volatiles were removed under vacuum and the residue was taken up in 70 ml 1N HCl. Extraction with ethyl acetate drying of the combined organic fractions and evaporation yielded a residue which was purified by reversed phase preparative HPLC eluting with an acetonitrile/water gradient. Evaporation of the product fractions yielded the title compound. MS (m/e): 297.0 (M−H, 100%)

来源