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Trimethyl orthoformate → 1-Bromo-2-(dimethoxymethyl)-4,5-dimethoxybenzene
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Trimethyl orthoformate | HCID 9005 | — |
| 反応物 | 6-Bromo-3,4-dimethoxybenzaldehyde | HCID 79351 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 1-Bromo-2-(dimethoxymethyl)-4,5-dimethoxybenzene | HCID 11077146 | — |
反応手順
6-Bromo-3,4-dimethoxybenzaldehyde (470 g) is suspended in methanol (600 ml), and thereto are added trimethyl orthoformate (1025 ml) and IRA-120 (H+ -type, 10 g), and the mixture is refluxed for one hour. The mixture is cooled to room temperature, and the insoluble materials are removed by filtration, and the filtrate is concentrated under reduced pressure. The resulting residue is dissolved in ether, washed, dried, evaporated to remove the ether, and distilled under reduced pressure to give 6-bromo-3,4-dimethoxybenzaldehyde dimethyl acetal (522 g) as a main distillate (133-138° C./1 Torr).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06005106 |
| 出典データセット | uspto-grants-1999_12 |
| ORD ID | ord-a4faae7e17ca4d15b79f5c74c0c70843 |
| 出典メモ | uspto-grants-1999_12 |