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Hydrochloric Acid → 2-Hydroxy-4,5-dimethoxybenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 2,4,5-Trimethoxybenzaldehyde | HCID 20525 | — |
| 反応物 | Boron Trichloride | HCID 25135 | — |
| 反応物 | Acetone cardice | HCID 18522661 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 2-Hydroxy-4,5-dimethoxybenzaldehyde | HCID 10986908 | 102.1% |
反応手順
A solution of boron trichloride (50 mL, 1.0 M solution in CH2Cl2) was slowly added to a solution of 2,4,5-trimethoxybenzaldehyde (3.92 g, 20 mmol) in CH2Cl2 (200 mL) at −78° C. (dry ice/acetone bath). The mixture was warmed to room temperature and stirred for three hours. 10 mL of HCl (37%) aqueous solution was poured into the resulting solution at 0° C. and extracted with CH2Cl2 (150 mL×3). The combined organic layer was washed with saturated aqueous NaCl (200 mL×2), water (100 mL×1), dried over MgSO4, and evaporated to afford 3.72 g of a light brown solid (3.72 g, 99%): 1H-NMR (400 MHz, CDCl3) δ3.88 (s, 3H), 3.94 (s, 3H), 6.47 (s, 1H), 6.91 (s, 1H), 9.70 (s, 1H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07262301B1 |
| 出典データセット | uspto-grants-2007_08 |
| ORD ID | ord-ff47265027314f2c8b0a1e87b2ead4b4 |
| 出典メモ | uspto-grants-2007_08 |