HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hypofluorous acid, trifluoromethyl ester → 3-fluoro-1,3-dihydro-7-nitro-5-phenyl-2H-1,4-benzodiazepin-2-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hypofluorous acid, trifluoromethyl ester | HCID 78989 | — |
| Reactant | 4-p-toluenesulfonyl-5-phenyl-7-nitro-2,3,4,5-tetrahydro-1H-1,4-benzodiazepin-2-one | HCID 23332655 | — |
| Reactant | 3-fluoro-4-p-toluenesulfonyl-5-phenyl-7-nitro-2,3,4,5-tetrahydro-1H-1,4-benzodiazepin-2-one | HCID 23332675 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 3-fluoro-1,3-dihydro-7-nitro-5-phenyl-2H-1,4-benzodiazepin-2-one | HCID 13125994 | — |
Reaction Steps
2.35 g. of sublimed potassium tert.-butylate are added at 5° to a solution of 4.55 g. of 3-fluoro-4-p-toluenesulfonyl-5-phenyl-7-nitro-2,3,4,5-tetrahydro-1H-1,4-benzodiazepin-2-one, obtainable from 4-p-toluenesulfonyl-5-phenyl-7-nitro-2,3,4,5-tetrahydro-1H-1,4-benzodiazepin-2-one and CF3OF, in 50 ml. of DMF. After stirring for 1 hour, the temperature is allowed to rise to 20° and the mixture is stirred for 48 hours more. The mixture is poured onto ice and worked up in the customary manner to give 3-fluoro-5-phenyl-7-nitro-2,3-dihydro-1H-1,4-benzodiazepin-2-one.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US04232016 |
| Source dataset | uspto-grants-1980_11 |
| ORD ID | ord-930db9717e944bd3a8b5d05a3ffb243a |
| Source note | uspto-grants-1980_11 |