HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 5-(2-chlorophenyl)-1,2,3,6,7,9-hexahydro-3-hydroxy-N-(4-methoxy-2-nitrophenyl)-2-oxo-1-(2-phenylethyl)-8H-pyrido[4',3':4,5]thieno[2,3-e]-1,4-diazepine-8-carbothioamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Methoxy-2-nitrophenyl isothiocyanate | HCID 141006 | — |
| Reactant | 5-(2-chlorophenyl)-1,2,3,6,7,9-hexahydro-3-hydroxy-1-(2-phenylethyl)-8H-pyrido[4',3':4,5]thieno[2,3-e]-1,4-diazepine-2-one | HCID 15887972 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 5-(2-chlorophenyl)-1,2,3,6,7,9-hexahydro-3-hydroxy-N-(4-methoxy-2-nitrophenyl)-2-oxo-1-(2-phenylethyl)-8H-pyrido[4',3':4,5]thieno[2,3-e]-1,4-diazepine-8-carbothioamide | HCID 15887973 | — |
Reaction Steps
5-(2-chlorophenyl)-1,2,3,6,7,9-hexahydro-3-hydroxy-1-(2-phenylethyl)-8H-pyrido[4′,3′:4,5]thieno[2,3-e]-1,4-diazepine-2-one (0.167 g, 0.29 mmol) is dissolved in dichloromethane (2 ml). Triethylamine (0.06 ml, 0.44 mmol) then 4-methoxy 2-nitrophenylisothiocyanate (0.062 g, 0.29 mmol) are added. After agitation at 23° C. for 2 hours, the solvent is evaporated off. After purification by chromatography on a silica column (eluent: dichloromehane-methanol: 98-2), the fractions contining only the product are evaporated. The solid is taken up in ether and a drop of dichloromethame and a drop of acetone are added. After filtration on flit and washing the solid with ether, the desired product is obtained in the form of a yellow powder (0.08 g, 41%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06777408B1 |
| Source dataset | uspto-grants-2004_08 |
| ORD ID | ord-4124d29d39784078bf0974d3ba775bc4 |
| Source note | uspto-grants-2004_08 |