反应详情

Triethylamine (0.5 ml) was added dropwise to a suspension of 3-pyridin-3-ylacrylic acid (5.0 g) in anhydrous dichloromethane (30 ml), and 6 ml of oxalyl chloride was added dropwise slowly in an ice-bath with the temperature no more than 5° C. After addition, the reaction was carried out for 30 min in an ice-bath, and then at room temperature overnight. The completion of reaction was indicated by TLC. The reaction mixture was concentrated under reduced pressure to give a white solid, which was left to stand at room temperature for 1 h, and used directly for the next step.

1. additionwas added dropwise slowly in an ice-bath with the temperature no more than 5° C
2. additionAfter addition
3. customat room temperature
4. customovernight
5. customThe completion of reaction
6. concentrationThe reaction mixture was concentrated under reduced pressure
7. customto give a white solid, which
8. waitwas left
9. waitto stand at room temperature for 1 h