HuagongsheHuagongshe Chemistry Print Report · For research reference only
Water → HCID 53655027, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Water | HCID 962 | — |
| Reactant | Chlorosuccinimide | HCID 31398 | — |
| Reactant | HCID 54105642 | HCID 54105642 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 53655027 | HCID 53655027 | — |
Reaction Steps
3 g (11 mmol) of (S)-7-chloro-11,12,13,13a-tetrahydro-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-9-one in 30 ml of dimethylformamide are stirred at 90° for 30 minutes with 1.60 g of N-chlorosuccinimide. The solution is poured into water and extracted with chloroform. The chloroform extracts are washed several times with water, dried over magnesium sulphate and evaporated. By chromatography on a silica gel column and subsequent recrystallization from ethyl acetate there is obtained (S)-1,7-dichloro-11,12,13,13a-tetrahydro-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepin-9-one of melting point 209°-210°.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04352818 |
| Source dataset | uspto-grants-1982_10 |
| ORD ID | ord-670758ee544147dca092b6627d31fe71 |
| Source note | uspto-grants-1982_10 |