HuagongsheHuagongshe Chemistry Print Report · For research reference only
1-Bromo-3-chloropropane → 3-(3-Chloropropyl)-1,3-dihydro-7,8-dimethoxy-2H-3-benzazepin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1-Bromo-3-chloropropane | HCID 8006 | — |
| Reactant | 1,3-Dihydro-7,8-dimethoxy-2H-3-benzazepin-2-one | HCID 1482373 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Solvent | Dimethyl Sulfoxide | HCID 679 | — |
| Product | 3-(3-Chloropropyl)-1,3-dihydro-7,8-dimethoxy-2H-3-benzazepin-2-one | HCID 13092503 | — |
Reaction Steps
Here, 7,8-dimethoxy-1,3-dihydro-2H-3-benzazepin-2-one (131.5 g, 0.6 mol) is suspended in dimethylsulfoxide (900 ml) and mixed with potassium tert.butoxide (80.8 g, 0.72 mol) with stirring. After 10 minutes, the solution obtained is added dropwise, while cooling with ice water, to 1-bromo-3-chloropropane (77 ml, 0.72 mol) in dimethylsulfoxide (300 ml). After 1 hour the mixture is poured into ice water. After a short time the greasy precipitate begins to crystalize. The precipitate is suction filtered, dissolved in acetone, precipitated with water once again, suction filtered and dried.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04737495 |
| Source dataset | uspto-grants-1988_04 |
| ORD ID | ord-da77e7dadbc34669b8085240581b845a |
| Source note | uspto-grants-1988_04 |