HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 53855886, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 2-Bromo-N-methyl-N-phenylacetamide | HCID 34495 | — |
| Reactant | HCID 135744107 | HCID 135744107 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 53855886 | HCID 53855886 | 39% |
Reaction Steps
80% Sodium hydride in oil (102 mg) was added to a solution of phenylmethyl [2,3-dihydro-5-methyl-2-oxo-1H-1,4-benzodiazepin-3-yl]carbamate (1.00 g) in dry DMF (10 ml) under nitrogen. The mixture was stirred for 0.5 h at 23° and was treated with a solution of 2-bromo-N-methyl-N-phenylacetamide (707 mg) in dry DMF (1 ml). The mixture was stirred at 23° for 1 h, partitioned between phosphate buffer solution (pH6.5) and EA, the organic phase was washed with water and dried. The solvent was evaporated in vacuo and the residue was purified by chromatography on alumina. Elution with MeOH-DCM (1:50) gave the title compound (568 mg).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05569654 |
| Source dataset | uspto-grants-1996_10 |
| ORD ID | ord-df6a8fce052d47c18f89938a28d045c4 |
| Source note | uspto-grants-1996_10 |