反应详情

To an ice-water cooled suspension of 211 mg of 2-methyl-N-[4-(5H-pyrrolo[2,1-c][1,4]-benzodiazepin-10(11H)-ylcarbonyl)-phenyl]benzamide in 5 ml of tetrahydrofuran is added 67 mg of N-chlorosuccinimide followed by continued stirring in the cold for 10 minutes. The bath is removed and stirring continued for 2.25 hours. The reaction mixture is added to ice-water and extracted with ether. The organic layer is dried and concentrated in vacuo to give a foam which is crystallized from ethyl acetate-hexane to give 157 mg of the desired product as an orange-pink solid, m.p. 185°-187° C.

1. customThe bath is removed
2. stirringstirring
3. waitcontinued for 2.25 hours
4. additionThe reaction mixture is added to ice-water
5. extractionextracted with ether
6. customThe organic layer is dried
7. concentrationconcentrated in vacuo
8. customto give a foam which
9. customis crystallized from ethyl acetate-hexane