化工社化工社 化学情報印刷レポート · 研究参考用
Hexamethylenetetramine → 3,5-Difluoro-4-hydroxybenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexamethylenetetramine | HCID 4101 | — |
| 反応物 | Trifluoroacetic acid | HCID 6422 | — |
| 反応物 | 2,6-Difluorophenol | HCID 94392 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 3,5-Difluoro-4-hydroxybenzaldehyde | HCID 10192584 | — |
反応手順
TFA (7 mL) was added to 2,6-difluoro-phenol (1.0 g, 7.69 mmol) and hexam-ethylenetetraamine (1.08 g, 7.69 mmol), and the mixture was stirred at 75˜80° C. for 12 hours. The reactant was cooled, diluted with water, and then extracted with DCM/MeOH (9:1) solution three or four times. The organic layer was concentrated under reduced pressure, and DCM was added to the residue. The mixture was dried with MgSO4 and concentrated under reduced pressure. The reaction product was used in the next step without a separate purification process.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09447044B2 |
| 出典データセット | uspto-grants-2016_09 |
| ORD ID | ord-027e21b1ee4d42b3bf74111e4af661b8 |
| 出典メモ | uspto-grants-2016_09 |