HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → HCID 9945554, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 4-Phenylbenzoyl chloride | HCID 84151 | — |
| Reactant | 5,6,7,8-Tetrahydro-4H-thieno[3,2-B]azepine | HCID 11804971 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 9945554 | HCID 9945554 | 75.1% |
Reaction Steps
A solution of 5,6,7,8-tetrahydro-4H-thieno[3,2-b]azepine of Step A (0.300 g) and N,N-diisopropylethyl amine (0.5 mL) in dichloromethane (25 mL) was cooled to 0°. To this was added a solution of 4-biphenyl carbonyl chloride (0.518 g) in dichloromethane (5 ml). The solution was stirred overnight as it warmed to room temperature, then washed with 0.1N hydrochloric acid, aqueous sodium bicarbonate and brine. The organic layer was dried over anhydrous sodium sulfate, filtered and evaporated to an oil. Flash chromatography of the residue on silica gel provided the title compound as a white solid (0.490 g), m.p. 164-166° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06903091B2 |
| Source dataset | uspto-grants-2005_06 |
| ORD ID | ord-d288369e67174533afc18075c92b1a3e |
| Source note | uspto-grants-2005_06 |