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 reaction was allowed to warm to room temperature with stirring overnight. The pyridine was removed under vacuum, added dichloromethane and water. Product precipitated as a grey solid and was washed with dilute hydrochloric acid, water and air dried. The dichloromethane layer was separated, washed with dilute hydrochloric acid, and water, dried over sodium sulfate (anh.) and solvent removed to give a total of 12.45 g product (77% yield).

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