تفاعل #2358485

معادلة التفاعل

2-fluoro-5-(trifluoromethyl)benzaldehyde

methyl thioglycolate

potassium carbonate

DMF

→

methyl 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylate

المردود 93.0%

المذيبات

water

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةthe reaction mixture was cooled to room temperature
2. 2
   استخلاصextracted with tert-butyl methyl ether 3 times
3. 3
   غسيلThe combined organic layer was washed with water
4. 4
   تجفيفThe mixture was dried over magnesium sulfate
5. 5
   تركيزconcentrated under reduced pressure
6. 6
   أخرىThe residue was recrystallized from methanol

الإجراء التجريبي

A mixture of 5.0 g of 2-fluoro-5-(trifluoromethyl)benzaldehyde, 3.3 g of methyl thioglycolate, 4.0 g of potassium carbonate and 50 ml of DMF was stirred at 60° C. for 2 hours, and then the reaction mixture was cooled to room temperature. To the reaction mixture was added water, and extracted with tert-butyl methyl ether 3 times. The combined organic layer was washed with water, followed by saturated aqueous sodium chloride solution. The mixture was dried over magnesium sulfate, and then concentrated under reduced pressure. The residue was recrystallized from methanol to obtain 6.3 g of methyl 5-(trifluoromethyl)benzo[b]thiophene-2-carboxylate (the present compound 1).

المصدر