HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dimethylamine → HCID 17848835, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dimethylamine | HCID 674 | — |
| Reactant | HCID 17848844 | HCID 17848844 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 17848835 | HCID 17848835 | — |
Reaction Steps
50% aqueous dimethylamine (27 ml) was added to a solution of 1-(1-acetyl-2,3,4,5-tetrahydro-1H-1-benzazepin-8-yl)-3-chloro-1-propanone (7.10 g, 25.4 mmol) obtained in Reference Example 7 in dichloromethane at room temperature, and then stirred for 4 hours. After the reaction solution was separated, the organic layer was washed with a saturated saline solution and dried over anhydrous sodium sulfate, and the solvent was distilled away under reduced pressure. The resultant residues were purified by alumina column chromatography (developing solvent; hexane:ethyl acetate=1:1) and crystallized from hexane, whereby the title compound (5.38 g) was obtained as colorless powder with a mp. of 68 to 70° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07229986B2 |
| Source dataset | uspto-grants-2007_06 |
| ORD ID | ord-9503d4a9877045dc967b4dbaed46cf2d |
| Source note | uspto-grants-2007_06 |