反应详情

温度

0 °C

2-Amino-thiophene-3-carboxylic acid amide (8.73 g, 61.4 mmole) was dissolved in pyridine (100 ml), cooled to 0° C., and 2-fluorobenzoyl chloride was added dropwise over 20 min, then the reaction was allowed to warm to room temperature with stirring overnight. The pyridine was removed under vacuum, dichloromethane and water were added. The product was precipitated as a grey solid and was washed with diluted hydrochloric acid, water and air dried. The dichloromethane layer was separated, washed with diluted hydrochloric acid, and water, dried over sodium sulfate (anh.) and the solvent was removed to give a total of 12.45 g product (77% yield).

1. temperatureto warm to room temperature
2. customThe pyridine was removed under vacuum, dichloromethane and water
3. additionwere added
4. customThe product was precipitated as a grey solid
5. washwas washed with diluted hydrochloric acid, water and air
6. customdried
7. customThe dichloromethane layer was separated
8. washwashed with diluted hydrochloric acid, and water
9. dry with materialdried over sodium sulfate (anh.)
10. customthe solvent was removed