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Hydrazine hydrate (1:1) → 4-Cyanobenzohydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | Ethyl 4-cyanobenzoate | HCID 81589 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-Cyanobenzohydrazide | HCID 456732 | 90.2% |
反応手順
To a 250 mL round bottom flask charged with ethyl 4-cyanobenzoate (16.85 g, 96.2 mmol) in 95% ethanol (75 mL) was added hydrazine mono-hydrate (18.2 mL, 64% solution, 240 mmol). This mixture was heated to reflux for a period of 4.5 h, then allowed to cool to room temperature over a 16 h period. The solvent was removed under reduced pressure and the yellow residue was taken up in ice-cold water (150 mL). The light yellow solid was filtered off and washed with additional cold water (50 mL). The solid was then dried under high vacuum to yield the title compound as a light yellow solid (13.98 g, 90%). 1H NMR (400 MHz, DMSO-d6, δ in ppm) 10.05 (br s, 1H) 7.95 (AA′XX′, J=8.5 Hz, 4H), 4.61 (br s, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08629167B2 |
| 出典データセット | uspto-grants-2014_01 |
| ORD ID | ord-c33ed2630b134739b0597c89be6a8d38 |
| 出典メモ | uspto-grants-2014_01 |