反应详情

In the manner of Example XI, part D, 7 g of 5-amino-3-(butylmethylamino)-4-cyanoisothiazole, 4.1 ml (4 g) of methyl isocyanate, and a catalytic amount of dibutyltin diacetate in 50 ml of tetrahydrofuran were allowed to react. The volatile materials were removed under reduced pressure and the residue was crystallized from 35 ml of 70:30 diethyl ether:hexane to yield solid material, mp 102° (decomposes). This material was recrystallized from 70 ml of 40:60 diethylether:hexane to yield 4.1 g of 1-methyl-3-(3-(butylmethylamino)-4-cyano-5-isothiazolyl)urea mp 169°-170°. The nmr spectrum was consistent with the assigned structure.

1. customto react
2. customThe volatile materials were removed under reduced pressure
3. customthe residue was crystallized from 35 ml of 70:30 diethyl ether
4. customhexane to yield solid material, mp 102° (decomposes)
5. customThis material was recrystallized from 70 ml of 40:60 diethylether