HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylformamide → HCID 54511176, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylformamide | HCID 6228 | — |
| Reactant | Benzyl Bromide | HCID 7498 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 54063239 | HCID 54063239 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 54511176 | HCID 54511176 | 90% |
Reaction Steps
Under nitrogen gas atmosphere and ice cooling, benzyl bromide (11.4 ml, 95.5 mmol) was added to a mixture of 60% sodium hydride (3.8 g, 95.5 mmol), Compound 11 (6.7 g, 19.1 mmol) and dimethylformamide (20 ml), and the mixture was stirred for 18 hours. Methanol was added to the reaction mixture under ice cooling and stirred for 1 hour, and the solvent was evaporated under reduced pressure. The residue was diluted with diethyl ether, washed successively with water and saturated brine, and dried over magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography (n-hexane:ethyl acetate=10:1-9:1) to obtain Compound 12 (9.1 g, 90%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06562954B1 |
| Source dataset | uspto-grants-2003_05 |
| ORD ID | ord-28c75ac2d2e449929cfa83cdb3050f63 |
| Source note | uspto-grants-2003_05 |