関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 4-Methoxybenzyl alcohol | HCID 7738 | — |
| 反応物 | 1,3-Dichloro-5,5-dimethylhydantoin | HCID 8360 | — |
| 反応物 | 4-Chloroanisole | HCID 12167 | — |
| 反応物 | Sodium Acetate | HCID 517045 | — |
| 触媒 | Tempo | HCID 2724126 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 4-Methoxybenzaldehyde | HCID 31244 | 91.1% |
反応手順
5 g (36.2 mmol) of anisyl alcohol, 3.0 g (36.6 mmol) of sodium acetate and 4.2 g (21.3 mmol) of dichlorodimethylhydantoin were suspended in 40 ml of methylene chloride in a 100 ml sulphonation flask. The suspension was cooled to 0° C. while stirring and treated with 10 mg (0.06 mmol) of TEMPO, whereupon the mixture was held at 0° C. for 16 hours. Thereafter, the reaction had finished without 4-chloro-anisole being formed in any amount worth mentioning. The white precipitate was filtered off and the filtrate was washed with sodium bicarbonate solution and with sodium chloride solution. Distillation of the crude product gave 4.49 g (91%) of anisaldehyde GC content: 88.8% (area percent).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05821374 |
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| 出典データセット | uspto-grants-1998_10 |
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| ORD ID | ord-7fb77186813d48168788ca19dfc8ce42 |
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| 出典メモ | uspto-grants-1998_10 |
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