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Iodine → Benzene, (diazomethyl)-
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Iodine | HCID 807 | — |
| 反応物 | Peracetic Acid | HCID 6585 | — |
| 反応物 | 1,1,3,3-Tetramethylguanidine | HCID 66460 | — |
| 反応物 | Benzylidene-hydrazine | HCID 95742 | — |
| 溶媒 | 1,2-Dichloroethane | HCID 11 | — |
| 生成物 | Benzene, (diazomethyl)- | HCID 136601 | — |
反応手順
To benzaldehyde hydrazone (5.95 g, 0.05 moles) in 1,2-dichloroethane (50 ml) containing 1,1,3,3-tetramethylguanidine (26.4 ml) and iodine (2 ml, 1% w/v solution) was added peracetic acid solution (11.4 ml, 1.27 × 0.05 moles) over 12 minutes at 0°. The red solution, which was gently evolving nitrogen, was stirred for 20 minutes at 0° to -5° before being washed with water (5 × 250 ml) and made up to 250 ml in a volumetric flask. An aliquot (50 ml) treated with excess acetic acid yielded 199 ml gas at NTP which corresponded to a yield of diazoalkane of 88.9%.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04083837 |
| 出典データセット | uspto-grants-1978_04 |
| ORD ID | ord-76870d5574c74ff6bf704d4e8a40f82b |
| 出典メモ | uspto-grants-1978_04 |