HuagongsheHuagongshe Chemistry Print Report · For research reference only
Bromine → Pyrrolo(3,4-e)-1,4-diazepin-2(1H)-one, 3,7-dihydro-8-bromo-6,7-dimethyl-5-phenyl-
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Bromine | HCID 24408 | — |
| Reactant | Premazepam | HCID 72104 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | Pyrrolo(3,4-e)-1,4-diazepin-2(1H)-one, 3,7-dihydro-8-bromo-6,7-dimethyl-5-phenyl- | HCID 3069503 | — |
Reaction Conditions
| Temperature | -60 °C |
|---|
Reaction Steps
3,7-dihydro-6,7-dimethyl-5-phenylpyrrolo[3,4-e][1,4]diazepin-2(1H)-one (5.0 g, 0.020 mole) is dissolved in methanol (150 ml) and the obtained solution is cooled to -60° C. and stirred during the addition of a solution of bromine (3.4 g, 0.021 mole) in methanol (10 ml). After 20 minutes at -60° C., the reaction mixture is poured into an aqueous solution of NaHCO3 (1.5% w/v, 750 ml). The precipitate which forms is recovered by filtration and crystallized from methanol yielding 4.2 g of the compound of the title. M.p. 200°-2° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04391817 |
| Source dataset | uspto-grants-1983_07 |
| ORD ID | ord-1eff709048cc4cb1aab4f5696b5ac5f4 |
| Source note | uspto-grants-1983_07 |