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p-Toluohydrazide → 4-Methyl-benzoic acid-(1-imino-ethyl)-hydrazide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | p-Toluohydrazide | HCID 77174 | — |
| 反応物 | Ethanimidic acid, ethyl ester, hydrochloride (1:1) | HCID 2724290 | — |
| 反応物 | Sodium | HCID 5360545 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-Methyl-benzoic acid-(1-imino-ethyl)-hydrazide | HCID 68495467 | 15.7% |
反応手順
1.65 g (72 mmol) sodium are dissolved in 80 mL ethanol. 8.89 g (72 mmol) ethyl acetimidate hydrochloride in 160 mL ethanol are added at ambient temperature and the precipitated sodium chloride is filtered off. The filtrate is combined with 6.00 g (40 mmol) 4-methyl-benzoic acid hydrazide and stirred overnight. The reaction mixture is evaporated down and cooled. The precipitated solid is filtered off and washed with cold ethanol and diethyl ether (5.7 g white solid). A further 1.2 g solid are obtained from the filtrate after distillation of the solvents and recrystallisation from ethanol.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07423036B2 |
| 出典データセット | uspto-grants-2008_09 |
| ORD ID | ord-7072e1c97cbd4655b956b63c85fe56c9 |
| 出典メモ | uspto-grants-2008_09 |