反应详情

A mixture of 1.41 g (0.0125 mole) of ethyl isocyanoacetate, 1.4 g (0.0125 mole) of potassium t-butoxide and 125 ml of tetrahydrofuran was stirred at room temperature for 10 minutes. Following the addition of 5.23 g (0.01 mole) of 7-chloro-5-(2-chlorophenyl)-2-[bis-(morpholino)-phosphinyloxy]-3H-1,4-benzodiazepine stirring was continued for 1/2 hr. The reaction mixture was acidified with glacial acetic acid, diluted with 250 ml of water and extracted with three 100 ml portions of methylene chloride. The methylene chloride extracts were washed with saturated sodium bicarbonate solution, dried and evaporated. The crystalline residue was collected and washed with ether to give product with mp 215°-220°. The material was recrystallized from methylene chloride/ethyl acetate for analysis, mp 225°-228°.

1. waitwas continued for 1/2 hr
2. extractionextracted with three 100 ml portions of methylene chloride
3. washThe methylene chloride extracts were washed with saturated sodium bicarbonate solution
4. customdried
5. customevaporated
6. customThe crystalline residue was collected
7. washwashed with ether
8. customto give product with mp 215°-220°
9. customThe material was recrystallized from methylene chloride/ethyl acetate for analysis, mp 225°-228°