Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HCID 14985095 | HCID 14985095 | — |
| Reactant | 10,11-Dihydro-5H-benzo[e]pyrrolo[1,2-a][1,4]diazepine | HCID 15547048 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 22405322 | HCID 22405322 | — |
Reaction Steps
To a stirred solution of 2.0 g of 10,11-dihydro-5H-pyrrolo[2,1-c][1,4]benzodiazepine in 30 ml of methylene chloride, under nitrogen, while cooling to 0° C. is added dropwise 30 ml of triethylamine followed by a solution of 4'-(propyl)[1,1'-biphenyl]-4-carbonyl chloride in 10 ml of methylene dichloride. The reactants are stirred at room temperature for 16 hours. The reaction mixture is poured in ice water and extracted with methylene chloride (3×50 ml) The organic layer is, washed with water, 2N citric acid, saturated aqueous NaHCO3, water and dried (MgSO4) and evaporated in vacuo to give a residue which is purified by column chromatography on silica gel with ethyl acetate-hexane to give 1.4 g of the desired product as a crystalline solid, m.p. 118°-120° C. MS(M+H=407.3; M+Na=429.3)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patent number | US05521173 |
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| Source dataset | uspto-grants-1996_05 |
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| ORD ID | ord-903ab17af4e748d1bd9e133ce898106e |
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| Source note | uspto-grants-1996_05 |
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