反应详情

温度

145 °C

A suspension of 8.0 g (51.5 mmol) of 2-mercaptonicotinic acid, 5.8 g (51.5 mmol) of 2-(aminomethyl)-thiophene and 3.5 g (25.8 mmol) of phosphorus trichloride in chlorobenzene (260 ml) was heated for 3 h under reflux (145° C.). When the reaction solution had cooled to 60° C., filtration with suction was carried out at that temperature. The solid obtained was taken up in a DCM/MeOH mixture (3:1, vv, 300 ml) and washed with water (2×50 ml). The organic phase was dried over MgSO4, filtered and concentrated in vacuo. Crystallization of the residue from ethyl acetate yielded 3.1 g (12.4 mmol, 24%) of 2-mercapto-N-(thiophen-2-ylmethyl)nicotinamide.

1. temperaturewas heated for 3 h
2. temperatureWhen the reaction solution had cooled to 60° C.
3. filtrationfiltration with suction
4. customThe solid obtained
5. washvv, 300 ml) and washed with water (2×50 ml)
6. dry with materialThe organic phase was dried over MgSO4
7. filtrationfiltered
8. concentrationconcentrated in vacuo
9. customCrystallization of the residue from ethyl acetate