反应 #2358487

ord-1d6e21acf49c416984f75fc425db3b8a

反应方程式

O=Cc1c(F)cccc1C(F)(F)F
2-fluoro-6-(trifluoromethyl)benzaldehyde
COC(=O)CS
methyl thioglycolate
O=C([O-])[O-].[K+].[K+]
potassium carbonate
CN(C)C=O
DMF
COC(=O)c1cc2c(C(F)(F)F)cccc2s1
methyl 4-(trifluoromethyl)benzo[b]thiophene-2-carboxylate
收率 35.4%

溶剂

反应条件

温度
130°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度The reaction mixture was cooled to room temperature
  2. 2
    萃取extracted with tert-butyl methyl ether 3 times
  3. 3
    洗涤The combined organic layer was washed with water
  4. 4
    干燥The mixture was dried over magnesium sulfate
  5. 5
    浓缩concentrated under reduced pressure

实验过程

A mixture of 1.00 g of 2-fluoro-6-(trifluoromethyl)benzaldehyde, 633 mg of methyl thioglycolate, 1.21 g of potassium carbonate and 15 ml of DMF was stirred at 130° C. for 2 hours. The reaction mixture was cooled to room temperature. To the reaction mixture was added water, and then 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 to obtain 480 mg of methyl 4-(trifluoromethyl)benzo[b]thiophene-2-carboxylate (the present compound 3).

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US09119396B2uspto-grants-2015_09