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Methyl 2-bromo-3-nitrobenzoate → 9-Nitro-1,2,3,4-tetrahydro-5H-1,4-benzodiazepin-5-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl 2-bromo-3-nitrobenzoate | HCID 79263 | — |
| 反応物 | Ethylenediamine monohydrate | HCID 12200817 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | 9-Nitro-1,2,3,4-tetrahydro-5H-1,4-benzodiazepin-5-one | HCID 2771611 | — |
反応手順
A mixture of 11.7 parts of methyl 2-bromo-3-nitrobenzoate, 8.1 parts of 1,2-ethanediamine monohydrate and 40 parts of 1-butanol was stirred for 1/2 hour at reflux temperature. The reaction mixture was evaporated and the residue was diluted with 50 parts of water. The precipitate was filtered off and washed with water and 2-propanol. It was then recrystallized from 2-methoxyethanol, yielding 6.5 parts of 2,3,4,5-tetrahydro-9-nitro-1H-1,4-benzodiazepin-5-one; mp. 191°-195° C. (interm. 1)
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05270464 |
| 出典データセット | uspto-grants-1993_12 |
| ORD ID | ord-6d2eab94fff14ac4bd1de5080b243cca |
| 出典メモ | uspto-grants-1993_12 |