HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethanol → 9-chloro-7-(2-chlorophenyl)-2-(methylthio)-5H-pyrimido[5,4-d][2]benzazepine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethanol | HCID 702 | — |
| Reactant | Dimethyl Sulfate | HCID 6497 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | 9-chloro-7-(2-chlorophenyl)-5H-pyrimido[5,4-d][2]benzazepine-2-thiol | HCID 178527848 | — |
| Solvent | Water | HCID 962 | — |
| Product | 9-chloro-7-(2-chlorophenyl)-2-(methylthio)-5H-pyrimido[5,4-d][2]benzazepine | HCID 13225513 | — |
Reaction Steps
A mixture of 1.1 g (3.0 mmole) of 9-chloro-7-(2-chlorophenyl)-5H-pyrimido[5,4-d][2]benzazepin-2-thiol, 1.0 ml (10 mmole) of dimethyl sulfate, 20 ml of 1N sodium hydroxide and 10 ml of ethanol was stirred at room temperature for 15 min. The mixture was diluted with water and extracted with methylene chloride. The methylene chloride solution was dried over anhydrous sodium sulfate and concentrated at reduced pressure to give an oil. Crystallization from ether gave colorless prisms, mp 187°-188° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04546183 |
| Source dataset | uspto-grants-1985_10 |
| ORD ID | ord-8afc0dedf7794f6d9ba1395a2f02990a |
| Source note | uspto-grants-1985_10 |