HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chloroethyl isocyanate → (+/-)-8-Methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-7-carboxylic acid (2-chloroethyl)-amide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chloroethyl isocyanate | HCID 16035 | — |
| Reactant | 1-(4-Nitrophenyl)-4-methyl-7,8-methylenedioxy-3,4-dihydro-5H-2,3-benzodiazepine | HCID 10336422 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | (+/-)-8-Methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine-7-carboxylic acid (2-chloroethyl)-amide | HCID 12137418 | 94.5% |
Reaction Steps
A mixture of 1.0 g (3.07 mmol) of (±)-8-methyl-5-(4-nitrophenyl)-8,9-dihydro-7H-1,3-dioxolo[4,5-h][2,3]benzodiazepine, 25 ml of dry dichloromethane and 0.62 g (5.88 mmol of 2-chloroethyl isocyanate was stirred at room temperature for 24 h, then concentrated. The residue was purified by refluxing in ethanol to yield 1.25 g (94%) of the title compound, Mp.: 222-223° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06858605B2 |
| Source dataset | uspto-grants-2005_02 |
| ORD ID | ord-2801449e76a54039a62ffd7aa20d7690 |
| Source note | uspto-grants-2005_02 |