反应详情

A solution of 3,4,6-trichloropyridazine (25 g) in tetrahydrofuran (200 ml) and triethylamine (19 ml) was treated at 0° C. (ice bath cooling) with 2-mercaptoethanol (8.33 ml) over 5 minutes: After the addition was complete, the mixture was stirred at rt for 72 hours. The mixture was stirred with aqueous sodium bicarbonate solution and DCM and the solid was collected, washed with water, ether and pentane and dried in vacuo, giving (22.9 g). The combined aqueous and organic fraction was evaporated to half volume giving further solid, which was washed and dried as above (5.0 g). The total yield of solid (27.9 g; 91%) contained some bromo-analogue (5-10%) by NMR.

1. additionAfter the addition
2. customthe solid was collected
3. washwashed with water, ether and pentane
4. customdried in vacuo
5. customgiving (22.9 g)
6. customThe combined aqueous and organic fraction was evaporated to half volume
7. customgiving further solid, which
8. washwas washed
9. customdried as above (5.0 g)