HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Bromo-2-Chloroethane → HCID 15542506, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Bromo-2-Chloroethane | HCID 7849 | — |
| Reactant | Ethyl Acetate | HCID 8857 | — |
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | HCID 15542509 | HCID 15542509 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 15542506 | HCID 15542506 | 42% |
Reaction Steps
50 mg of 7-chloro-4,5-dihydro-1,4-benzoxazepin-5-one was dissolved in dimethylformamide (1 ml), then 12 mg (1.2 equivalents) of 60% sodium hydride was added under ice cooling. This was agitated for 30 minutes, then 54 mg (1.5 equivalents) of 1-bromo-2-chloroethane was added and the result was agitated at room temperature for 10 hours. Ice water was added to the reaction solution, and extraction was performed by ethyl acetate. This ethyl acetate extract was washed by saline and was dried with anhydrous magnesium sulfate. The solvent was distilled off and the resultant crude product was refined with silica gel column chromatography (hexane:ethyl acetate 4:1) to obtain the above-referenced compound in an amount. of 28 mg (yield of 42%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06187769B1 |
| Source dataset | uspto-grants-2001_02 |
| ORD ID | ord-76c2627dafd94887a89898c11eb5a282 |
| Source note | uspto-grants-2001_02 |