HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methyl iodide → (Z)-8-bromo-1-methyl-5-phenyl-1H-benzo[e][1,4]diazepin-2(3H)-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methyl iodide | HCID 6328 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | (Z)-8-bromo-5-phenyl-1H-benzo[e][1,4]diazepin-2(3H)-one | HCID 59783468 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | (Z)-8-bromo-1-methyl-5-phenyl-1H-benzo[e][1,4]diazepin-2(3H)-one | HCID 59783784 | 60% |
Reaction Steps
Title compound 354 (3.1 g, 11.8 mmol), sodium hydride (565 mg, 14.14 mmol) and methyliodide (0.88 mL, 14.14 mmol) were stirred together in DMF (60 mL) at room temperature for 6 hours. DMF was removed and the residue was partitioned in EtOAc and water. The organic layer was dried, filtered and evaporated. The crude product was purified by flash chromatography (3:1 to 1:2 hexane:ethyl acetate) to afford title compound 357 (2.3 g, 60%) as a white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09193749B2 |
| Source dataset | uspto-grants-2015_11 |
| ORD ID | ord-6bafc14a28d44c55adb1d05e4e83e368 |
| Source note | uspto-grants-2015_11 |