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Dimethyl Sulfate → 2,3-Dimethoxy-6-nitrobenzaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Dimethyl Sulfate | HCID 6497 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Potassium | HCID 5462222 | — |
| 反応物 | 2-Hydroxy-3-methoxy-6-nitrobenzaldehyde potassium salt | HCID 86741192 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 2,3-Dimethoxy-6-nitrobenzaldehyde | HCID 7172127 | 80% |
反応手順
2-Hydroxy-3-methoxy-6-nitrobenzaldehyde potassium salt was slurried in acetone (500 mL) containing potassium carbonate (50 g) and the suspension was treated with dimethylsulfate (18.5 mL) and heated to reflux for one hour. An additional aliquot (18.5 mL) of dimethylsulfate was then added and the mixture was heated overnight. After 24 hours the red color of the potassium salt was virtually absent. The salts were removed by filtration, the filtrate was concentrated and the residue was recrystallized from isopropanol to give the title compound 40.0 g (80% from 3) mp 109°-110° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04751304 |
| 出典データセット | uspto-grants-1988_06 |
| ORD ID | ord-fdb1135aa64f479b9d5ffa1f9f79fafb |
| 出典メモ | uspto-grants-1988_06 |