HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 44212555, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 3-Cyclohexene-1-carbonyl chloride | HCID 523058 | — |
| Reactant | 5-(4-Aminobenzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine | HCID 15410467 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 44212555 | HCID 44212555 | 67.1% |
Reaction Steps
A mixture of 208 mg of 3-cyclohexene-1-carbonyl chloride (prepared from 3-cyclohexene-1-carboxylic acid and thionyl chloride) and 145 mg of triethylamine in 3 ml of methylene chloride is added to a solution of 377 mg of 5-(4-aminobenzoyl)-6,11-dihydro-5H-dibenz[b,e]azepine in 7 ml of methylene chloride. The mixture is stirred for 18 hours, washed with water, 1N HCl, water, 1M NaHCO3 and brine then dried with Na2SO4. The organic layer is passed through a short column of hydrous magnesium silicate and hexane added to the filtrate at the boil to give 340 mg of the desired product as a crystalline solid, m.p. 234°-236° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05869483 |
| Source dataset | uspto-grants-1999_02 |
| ORD ID | ord-5eb76c8903734231aafe0324a478531b |
| Source note | uspto-grants-1999_02 |