関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Dimethylamine | HCID 674 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 6-Chloroindole | HCID 87111 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 6-Chlorogramine | HCID 245814 | — |
反応手順
The starting material is prepared as follows: To the solution of 265 ml of acetic acid, 116 ml of 36% aqueous formaldehyde and 190 ml of 40% aqueous dimethylamine, 226.5 g of 6-chloroindole are added portionwise during 45 minutes while stirring at about 40°. The mixture is heated to 60° for 15 minutes and stirred at room temperature for 1 hour. It is cooled to 10°, combined with 500 ml of water, 400 ml of 25% aqueous sodium hydroxide and 100 ml of 20% aqueous sodium carbonate, stirred for 1/2 hour at 10°-20°, and filtered. The filtrate is combined with 250 ml 12% aqueous sodium carbonate, stirred for 1/2 hour, again filtered, both residues are washed with about 3 lt of water, combined and dried, to yield 300 g of 6-chloro-3-dimethylaminomethylindole melting at 130°-133°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04147786 |
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| 出典データセット | uspto-grants-1979_04 |
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| ORD ID | ord-0207170c5f784660be117c6afe2b44a9 |
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| 出典メモ | uspto-grants-1979_04 |
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