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N-Benzyl-N-nitroso-p-toluenesulfonamide → Benzene, (diazomethyl)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-Benzyl-N-nitroso-p-toluenesulfonamide | HCID 4118076 | — |
| 反応物 | Sodium Methoxide | HCID 10942334 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | tert-Butyl methyl ether | HCID 15413 | — |
| 生成物 | Benzene, (diazomethyl)- | HCID 136601 | 30% |
反応手順
N-Nitroso-N-benzyl-p-toluene sulphonamide (966 mg, 3.33 mmol) was added in small portions to a solution of sodium methoxide (2.0 ml of 2M solution in methanol) in t-butyl methyl ether (12 ml) and methanol (2 ml) at room temperature. After the addition was finished the reaction mixture was refluxed for 15-30 min. The reaction mixture was cooled and washed with water (3×6 ml). The ethereal solution of phenyl diazomethane was dried over sodium sulphate for 30 minutes. The solvent was removed in vacuo and the residue distilled under reduce pressure to give phenyl diazomethane as a dark red oil (30% yield, b.p. 20° C. at 1 mmHg) which was immediately dissolved in t-butyl methyl ether (6 ml).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05703246 |
| 出典データセット | uspto-grants-1997_12 |
| ORD ID | ord-f49d6f158adc41dfba6332ceeb0af4e9 |
| 出典メモ | uspto-grants-1997_12 |