反应详情

A mixture of 2-chloro-4,6-dimethylnicotinonitrile (800 mg, 4.83 mmol) and thiourea (1.2 kg, 15.76 mmol) was heated at reflux (118° C.) in n-butanol for 4 h. After cooling to room temperature, the yellow solution turned to a suspension containing light yellow solids. The solids were collected by filtration, rinsed with n-butanol, and dried in vacuo to give 2-mercapto-4,6-dimethylnicotinonitrile (778 mg, 98% yield). C8H8N2S; light yellow powder; mp 219-221° C.; 1H NMR (400 MHz, CDCl3) δ 6.40 (1H, s), 2.45 (3H, s), 2.43 (3H, s); ESI-HRMS (negative mode) calcd for C8H7N2S: 163.0330. found: m/z 163.0332 [M−H]−.

1. temperaturewas heated
2. additioncontaining light yellow solids
3. filtrationThe solids were collected by filtration
4. washrinsed with n-butanol
5. customdried in vacuo