化工社化工社 化学情報印刷レポート · 研究参考用
Hydrochloric Acid → 2,3-Dihydroxy-4-methoxybenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Boron Trichloride | HCID 25135 | — |
| 反応物 | 2,3,4-Trimethoxybenzaldehyde | HCID 75006 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2,3-Dihydroxy-4-methoxybenzaldehyde | HCID 11557352 | 73% |
反応手順
A dry CH2Cl2 (200 mL) solution of 2,3,4-trimethoxybenzaldehyde (19.6 g, 100 mmol), under nitrogen, was stirred for 10 min and BCl3 (1.0M solution in CH2Cl2, 200 mL) was added. The reaction was stirred for 24 hours and a 10% sodium bicarbonate solution (40 g/360 mL) was added. The resulting solution was acidified with concentrated HCl to PH 1. The organic layer was separated, and the aq. layer was extracted with EtOAc (4×100 mL). The organic layer was dried with MgSO4 and filtered through celite. After solvent evaporation, the crude mixture was recrystallized using (Hexanes/EtOAc:70/30) to afford 12.2 g (72.6 mmol, 73%) of a purple solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07091240B2 |
| 出典データセット | uspto-grants-2006_08 |
| ORD ID | ord-9c5bd52821714c9bb9e8153a9d33262f |
| 出典メモ | uspto-grants-2006_08 |