反应详情

A mixture of 4,6-dichloropyrimidine-5-amine (E-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 resulting mixture is allowed to cool to RT and then concentrated in vacuo. The residue is poured into aqueous NaOH solution (200 mL, 1 M) and then neutralized with acetic acid to adjust the pH value 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 (E-3).

1. temperatureat reflux for 3 h
2. concentrationconcentrated in vacuo
3. additionThe residue is poured into aqueous NaOH solution (200 mL, 1 M)
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