反应详情

5-Amino-2-(3-cyano-1-pyrrolyl)fluorobenzene (4.6 g, 22.9 mmol) was stirred in dry pyridine (50 ml) 0°. Ethyl chloroformate (2.66 g, 24.5 mmol) was added, and stirring continued for 20 minutes at the same temperature before allowing the temperature to rise to ambient over 2 hours. Solvent was evaporated, the residue treated with iced water (50 ml), filtered off, and dried. Crystallisation of the crude product from ethanol (200 ml) gave the title product (4.9 g) mp 188-190°.

1. waitto ambient over 2 hours
2. customSolvent was evaporated
3. additionthe residue treated with iced water (50 ml)
4. filtrationfiltered off
5. customdried
6. customCrystallisation of the crude product from ethanol (200 ml)