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Hypofluorous acid, trifluoromethyl ester → 3-fluoro-1,3-dihydro-7-nitro-5-phenyl-2H-1,4-benzodiazepin-2-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hypofluorous acid, trifluoromethyl ester | HCID 78989 | — |
| 反応物 | 4-p-toluenesulfonyl-5-phenyl-7-nitro-2,3,4,5-tetrahydro-1H-1,4-benzodiazepin-2-one | HCID 23332655 | — |
| 反応物 | 3-fluoro-4-p-toluenesulfonyl-5-phenyl-7-nitro-2,3,4,5-tetrahydro-1H-1,4-benzodiazepin-2-one | HCID 23332675 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 3-fluoro-1,3-dihydro-7-nitro-5-phenyl-2H-1,4-benzodiazepin-2-one | HCID 13125994 | — |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04232016 |
| 出典データセット | uspto-grants-1980_11 |
| ORD ID | ord-930db9717e944bd3a8b5d05a3ffb243a |
| 出典メモ | uspto-grants-1980_11 |