HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 21249956, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Cyclopropanecarbonyl chloride | HCID 77637 | — |
| Reactant | HCID 21249960 | HCID 21249960 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 21249956 | HCID 21249956 | 93% |
Reaction Steps
0.69 g (1.77 mmol) of 7-bromo-8-methoxy-4-methyl-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine (Example 4, Step A) is acylated in methylene chloride (15 ml) in the presence of 0.29 ml (2.1 mmol) of triethylamine with 0.19 ml (2.1 mmol) of cyclopropanoic acid chloride at room temperature for 1.5 hours. After concentration by evaporation and suspension with water, 0.78 g of a crude product, which is purified by suspension in hot ethanol, is obtained. 0.75 g (93%) of 7-bromo-3-cyclopropylcarbonyl-8-methoxy-4-methyl-1-(4-nitrophenyl)-4,5-dihydro-3H-2,3-benzodiazepine with a melting point of 194-196° C. is obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06200970B1 |
| Source dataset | uspto-grants-2001_03 |
| ORD ID | ord-7c60cf63ded243b0bfd61274c4f0a350 |
| Source note | uspto-grants-2001_03 |