関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Dimethylsulphamoyl chloride | HCID 83372 | — |
| 反応物 | 2-Hydroxy-4,5-dimethoxybenzaldehyde | HCID 10986908 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Formyl-4,5-dimethoxyphenyl dimethylsulphamate | HCID 86643008 | 83% |
反応手順
Dissolve 16.2 g (0.0889 mol) of 3,4-dimethoxy-6-hydroxybenzaldehyde in 80 ml of DMF. Cool to 10° C. and add in portions 24.6 g (0.178 mol) of potassium carbonate. Allow to return to ambient temperature and stir for 30 minutes. Cool to approximately 10° C. and pour in dropwise 10.1 ml (0.093 mol) of N,N-dimethylsulphamoyl chloride. Allow to return to ambient temperature and stir for 2 h. Pour the reaction mixture into 600 g of water and ice and stir for 1 h at ambient temperature. The precipitate formed is filtered off and washed 3 times with 50 ml of water each time and then dried in vacuo. 21.3 g of title product are obtained.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08097720B2 |
|---|
| 出典データセット | uspto-grants-2012_01 |
|---|
| ORD ID | ord-c010bd7aa97d4a2297e58994385f2b9a |
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| 出典メモ | uspto-grants-2012_01 |
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