HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sulfuric Acid → 6-chloro-2,3,4,5-tetrahydro-7,8-dimethoxy-1-(4-methoxyphenyl)-1H-3-benzazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sulfuric Acid | HCID 1118 | — |
| Reactant | N-[2-Hydroxy-2-(4-methoxyphenyl)ethyl]-2-(2-chloro-3,4-dimethoxyphenyl)ethylamine | HCID 3018199 | — |
| Solvent | Trifluoroacetic acid | HCID 6422 | — |
| Product | 6-chloro-2,3,4,5-tetrahydro-7,8-dimethoxy-1-(4-methoxyphenyl)-1H-3-benzazepine | HCID 6455448 | 83.5% |
Reaction Steps
7.87 g of N-[2-hydroxy-2-(4-methoxyphenyl)ethyl]-2-(2-chloro-3,4-dimethoxyphenyl)ethylamine was dissolved in 59 ml of CF3COOH. 1.7 ml of concentrated H2SO4 was added to the solution and the reaction was conducted for 4 hours. After the completion of the reaction followed by concentration under reduced pressure, 100 ml of CHCl3 and 50 ml of 10% NaOH were added to the residue to conduct extraction. The extract was washed with water, dehydrated over MgSO4 and concentrated to dryness under reduced pressure to obtain 6.25 g (yield: 83.5%) of 6-chloro-2,3,4,5-tetrahydro-7,8-dimethoxy-1-(4-methoxyphenyl)-1H-3-benzazepine.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05292521 |
| Source dataset | uspto-grants-1994_03 |
| ORD ID | ord-9cf2b4aea8284db2b40d8336ca073cb3 |
| Source note | uspto-grants-1994_03 |