反应详情

A mixture of 20 mL of thionyl chloride and 0.243 g (0.001 mol) of 2′-(cyanomethyl)-1,1′-biphenyl-4-carboxylic acid of Step A was heated under reflux for 1 hour. The excess thionyl chloride was removed in vacuo. To the residue was added 35 mL of dry 1,4-dioxane, 0.318 g (0.001 mol) of N-(pyridin-3-ylmethyl)-10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine-3-carboxamide and 0.122 g (0.001 mol) of N,N-dimethylformamide. The reaction was heated under reflux for three hours, cooled and evaporated to dryness. The residue was collected, washed with water and triturated with ether to give 0.62 g. of a tan solid, m.p. 105-108° C.

1. temperaturewas heated
2. temperatureunder reflux for 1 hour
3. customThe excess thionyl chloride was removed in vacuo
4. temperatureThe reaction was heated
5. temperatureunder reflux for three hours
6. temperaturecooled
7. customevaporated to dryness
8. customThe residue was collected
9. washwashed with water
10. customtriturated with ether
11. customto give 0.62 g