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Formaldehyde → 2-Methyl-6-dimethylaminoethylpyrazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | 2,6-Dimethylpyrazine | HCID 7938 | — |
| 反応物 | Dimethylamine, hydrochloride | HCID 10473 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Methyl-6-dimethylaminoethylpyrazine | HCID 54495966 | 32.9% |
反応手順
A mixture of 2,6-dimethylpyrazine (Pyrazine Specialities, Inc., Atlanta, Georgia, containing 2%, 2,5-isomer) (15.5 g) and dimethylamine hydrochloride (13.0 g) was heated until it began refluxing, and then formaldehyde (22.5 g as 38% aqueous solution) was added over a 30-min period. The resulting solution was refluxed for 2 hours. The solution was cooled to room temperature and diluted with water, made basic by the addition of 10% aqueous solution of sodium hydroxide, and extracted with chloroform. After removing the solvent, distillation of the residue gave 7.8 g of 2-methyl-6-dimethylaminoethylpyrazine with 5% of the 2,5-isomer (33% yield), 120°-126° C./12 mm Hg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04992268 |
| 出典データセット | uspto-grants-1991_02 |
| ORD ID | ord-78f54b2a0a8d4c83848f75557bac25cb |
| 出典メモ | uspto-grants-1991_02 |