関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Formaldehyde | HCID 712 | — |
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | 2-Dimethylaminomethyl-3-methylfuran | HCID 10034749 | — |
| 触媒 | Zincchloride | HCID 3007855 | — |
| 生成物 | 2-Chloromethyl-5-dimethylaminomethyl-3-methylfuran | HCID 20402036 | — |
反応手順
To a solution of 2-dimethylaminomethyl-3-methylfuran (6.5 g; 37.0 mmoles) [prepared in Step A] in 250 ml of chloroform was added paraformaldehyde (1.67 g; 55.7 mmoles) and zinc chloride (312 mg), and a slow stream of HCl gas was bubbled through while stirring at ambient temperature for 15 minutes. Stirring was continued for 2 hours, then HCl gas was bubbled through for 15 minutes and the mixture stirred for 1 hour. At this time additional paraformaldehyde (1.67 g; 55.7 mmoles) was added to the reaction mixture and a slow stream of HCl gas was passed through for 15 minutes. After stirring at ambient temperature for 18 hours, the reaction mixture was filtered through Celite and the filtrate evaporated under reduced pressure to yield the title compound (4.97 g) which crystallized upon standing and was used without further purification in Step C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04380639 |
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| 出典データセット | uspto-grants-1983_04 |
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| ORD ID | ord-17c89b0b8bc240afb413485fcba6c4a5 |
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| 出典メモ | uspto-grants-1983_04 |
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