تفاعل #1810822

معادلة التفاعل

2-chloro-5-methanesulfonyl-benzoic acid

2,2,2-trifluoro-ethanol

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title compound

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

المذيبات

NEt3

ظروف التفاعل

المعالجة

1. 1
   أخرىThe volatiles were removed under vacuum
2. 2
   استخلاصExtraction with ethyl acetate
3. 3
   أخرىdrying of the combined organic fractions and evaporation
4. 4
   أخرىyielded a residue which
5. 5
   أخرىwas purified by reversed phase preparative HPLC
6. 6
   غسيلeluting with an acetonitrile/water gradient
7. 7
   أخرىEvaporation of the product fractions

الإجراء التجريبي

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%)

المصدر