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N'-Benzylidene-4-methylbenzene-1-sulfonohydrazide → Benzene, (diazomethyl)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N'-Benzylidene-4-methylbenzene-1-sulfonohydrazide | HCID 277551 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | Benzene, (diazomethyl)- | HCID 136601 | — |
反応手順
In an oven-dried round bottom flask was placed benzaldehyde tosylhydrazone (1.15 g, 4.2 mmol), followed by 4.3 mL of a 1.0M solution of sodium methoxide in methanol (2.3 g Na metal dissolved in absolute methanol and diluted to 100 mL). The mixture was swirled until all the contents dissolved. Most of the solvent was removed via romy evaporation and the last traces of solvent by evacuation of the flask under high vacuum for 2 hours. The solid obtained was subjected to a Kugelrohr distillation at 215° C. and 200 millitorr for 1 hour. At 68-70° C., the title compound, as a red oil, was collected in a receiver flask in a quantitative yield.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06124281 |
| 出典データセット | uspto-grants-2000_09 |
| ORD ID | ord-85a84420acbd433fa7065761804ed02b |
| 出典メモ | uspto-grants-2000_09 |