HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 7,8-Dimethoxy-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carbonyl chloride
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Diphosgene | HCID 10426 | — |
| Reactant | 7,8-Dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepine | HCID 12923429 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 7,8-Dimethoxy-1,2,4,5-tetrahydro-3H-3-benzazepine-3-carbonyl chloride | HCID 86628628 | — |
Reaction Steps
To 1.2 mL (10 mmol/1 eq.) of diphosgene in 20 mL of dichloromethane, at about 0° C., there are added, dropwise, a solution of 3.55 g (20 mmol) of 7,8-dimethoxy-2,3,4,5-tetrahydro-1H-3-benzazepine in 22 mL of dichloromethane, and then 4.2 mL (30 mmol/1.5 eq.) of triethylamine. Stirring overnight at ambient temperature and then concentration are carried out. The residue is taken up in dichloromethane, washed with water and dried over magnesium sulphate to yield, after concentration, the desired product.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08076325B2 |
| Source dataset | uspto-grants-2011_12 |
| ORD ID | ord-e3fb737e68f447fc86c7a2affe197dae |
| Source note | uspto-grants-2011_12 |