HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetyl chloride → 4-Acetyl-7-bromo-2,3,4,5-tetrahydro-3-(phenylmethyl)-1H-1,4-benzodiazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetyl chloride | HCID 6367 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 7-Bromo-2,3,4,5-tetrahydro-1-(1H-imidazol-4-ylmethyl)-4-(1-naphthalenylcarbonyl)-1H-1,4-benzodiazepine, hydrochloride | HCID 178479667 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-Acetyl-7-bromo-2,3,4,5-tetrahydro-3-(phenylmethyl)-1H-1,4-benzodiazepine | HCID 18422944 | — |
Reaction Conditions
| Temperature | 0 °C |
|---|
Reaction Steps
A mixture of Compound B (200 mg, 0.63 mmol), dichloromethane (5 mL), and aqueous sodium hydroxide (1 ml, 1N) was combined and cooled to 0° C. Acetyl chloride (66 mL, 0.94 mmol) was added to the mixture, and after stirring for 2 hour at 0° C. aqueous sodium hydroxide (20 ml, 1N) and dichloromethane (50 mL) were added, followed by extraction with dichloromethane (50 mL). The organic portions were combined, dried (Na2SO4), and concentrated to a crude oil (230 mg, 100%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06011029 |
| Source dataset | uspto-grants-2000_01 |
| ORD ID | ord-03212e6f4f9d4f2a982092799ff1dbf5 |
| Source note | uspto-grants-2000_01 |