HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium hydride → HCID 21455248, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium hydride | HCID 24758 | — |
| Reactant | 1-(2-Chloroethyl)pyrrolidine hydrochloride | HCID 81668 | — |
| Reactant | 4,9-Dihydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one | HCID 12521642 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 21455248 | HCID 21455248 | — |
Reaction Steps
A mixture of 0.31 g. of 55% sodium hydride-mineral oil dispersion and 0.60 g. of N-(2-chloroethyl)pyrrolidine hydrochloride in 25 ml. of dry dimethylformamide is stirred at room temperature for 0.5 hours. To the mixture is added 0.40 g. of 4,9-dihydro-4-methyl-10H-thieno[3,4-b][1,5]benzodiazepin-10-one and stirring is continued for 18 hours. The reaction mixture is cooled, quenched with water, and extracted with chloroform. The dried chloroform extracts are concentrated to an oil which crystallizes on trituration with ether. Recrystallization from ethyl acetate-hexane gives white crystals, m.p. 139°-141° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04007272 |
| Source dataset | uspto-grants-1977_02 |
| ORD ID | ord-39eef77769c1413e9dc57de04366871e |
| Source note | uspto-grants-1977_02 |