HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloride → HCID 19864281, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloride | HCID 312 | — |
| Reactant | HCID 19864278 | HCID 19864278 | — |
| Catalyst | Copper | HCID 23978 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 19864281 | HCID 19864281 | — |
Reaction Steps
Anhydrous copper I chloride (0.68 g) was added to a stirred solution of 3-bromo-6-methyl-8-phenyl-5,6,7,8-tetrahydro-4H-thieno[2,3-d]azepine (1.0 g) in dry dimethylformamide under nitrogen. The mixture was heated to 120° for 5 hours, evaporated, water added and extracted with dichloromethane. The extracts were dried, filtered and evaporated and the residue chromatographed on silica, eluting with 1% methanol in dichloromethane, to give a crude product which contained 10% of the starting bromo- compound. Further purification using preparative reverse phase high pressure liquid chromatographed gave the pure title product, m.p. 67° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04904653 |
| Source dataset | uspto-grants-1990_02 |
| ORD ID | ord-8f09f93c84e94ace87c1186d59ddd12e |
| Source note | uspto-grants-1990_02 |