反应详情

A mixture of 10.6g. (0.035 mole) of [4-(p-chlorobenzylamino)-6-methyl-2-pyrimidinylthio]acetonitrile, 4.83 g. (0.07 mole) of hydroxylamine hydrochloride and 14.7 g. (0.14 mole) of sodium carbonate in 100 ml of N,N-dimethylformamide was heated on a steam bath for 3 hours. The mixture was filtered and the filtrate evaporated in a rotary-evaporator. The residue was triturated with petroleum ether containing a little ethyl acetate. The solid which crystallized was collected and recrystallized from ethyl acetate to give pure free base, m.p. 113°-116°. This free base was dissolved in absolute ethanol and acidified with an ethereal hydrochloric acid solution to give 3.5 g. of product, as the dihydrochloric salt, m.p. 230°-232° d.

1. additionA mixture of 10.6g
2. filtrationThe mixture was filtered
3. customthe filtrate evaporated in a rotary-evaporator
4. customThe residue was triturated with petroleum ether containing a little ethyl acetate
5. customThe solid which crystallized
6. customwas collected
7. customrecrystallized from ethyl acetate
8. customto give pure free base, m.p. 113°-116°
9. customto give 3.5 g