HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → N-[4-[(Dibenz[b,f] [1,4]thiazepin-10(11H)-yl)carbonyl]phenyl]-2,4-dichlorobenzamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,4-Dichlorobenzoyl chloride | HCID 66645 | — |
| Reactant | 10,11-Dihydro-10-(4-aminobenzoyl)dibenz[b,f][1,4]thiazepine | HCID 54230002 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-[4-[(Dibenz[b,f] [1,4]thiazepin-10(11H)-yl)carbonyl]phenyl]-2,4-dichlorobenzamide | HCID 67625596 | 78.9% |
Reaction Steps
To a solution of 452 mg of 2,4-dichlorobenzoyl chloride in 6 ml of methylene chloride is added 0.6 g of 10-(4-aminobenzoyl)-10,11-dihydrodibenz[b,f]-[1,4]thiazepine followed by 0.375 ml of triethylamine. The reaction mixture is stirred at room temperature for 18 hours. The reaction mixture is washed with 20 ml of water, 1 N HCl, 1N Na2CO3, water and dried over MgSO4. The filtrate is evaporated in vacuo to give 0.72 g of yellowish solid which is purified by silica gel chromatography on thick layer plates by elution with 1:1 ethyl acetate-hexane to give 0.254 g of the desired product as ivory crystals, m.p. 112°-115° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05686445 |
| Source dataset | uspto-grants-1997_11 |
| ORD ID | ord-10136550f8e542e1827723df9f032423 |
| Source note | uspto-grants-1997_11 |