HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 21467152, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,4-Dichlorobenzoyl chloride | HCID 66645 | — |
| Reactant | (4-Aminophenyl)(2-chloro-5,6,7,8-tetrahydro-4H-thieno[3,2-b]azepin-4-yl)methanone | HCID 21467127 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 21467152 | HCID 21467152 | 82.1% |
Reaction Steps
To a cooled (ice bath) solution of 0.245 g (0.8 mmol) of 2-chloro-4-(4-aminobenzoyl)-5,6,7,8-tetrahydro-4H-thieno[3,2-b]azepine and 167 μl (1.2 mmol) of triethylamine in 5 ml of dichloromethane is added 140 μl (1 mmol) of 2,4-dichlorobenzoyl chloride. The solution is stirred under argon at room temperature overnight and diluted with 60 ml of dichloromethane. The mixture is washed with 20 ml each of 2N-citric acid, H2O, 1M NaHCO3, brine and dried (Na2SO4). The solvent is removed and the residue crystallized from ethyl acetate-hexane to give 0.315 g of white crystals, m.p. 187°-189° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05654297 |
| Source dataset | uspto-grants-1997_08 |
| ORD ID | ord-12e34504bfaa4e92bfdaefab5c1047f3 |
| Source note | uspto-grants-1997_08 |