反应详情

The mixture of 4,6-dichloropyrimidine-5-amine (A-2) (16.0 g, 98.2 mmol) and sodium hydrosulphide (7.15 g, 128 mmol) in MeOH (320 mL) is stirred at reflux for 3 h. The reaction is complete based on TLC analysis. The reaction mixture is allowed to cool to RT and then concentrated in vacuo. The residue is poured into aqueous NaOH solution (1M, 200 mL) and then neutralized with acetic acid to adjust the pH to 5-6. The resulting mixture is stirred at RT for 30 min. The solid is collected by filtration, rinsed with water (2×50 mL) and dried in vacuo to afford the product, 5-amino-6-chloropyrimidine-4-thiol (A-3).

1. temperatureat reflux for 3 h
2. concentrationconcentrated in vacuo
3. additionThe residue is poured into aqueous NaOH solution (1M, 200 mL)
4. stirringThe resulting mixture is stirred at RT for 30 min
5. filtrationThe solid is collected by filtration
6. washrinsed with water (2×50 mL)
7. customdried in vacuo