関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | 4-Methylbenzyl chloride | HCID 7722 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 3-hydroxyimino-2-methoxyimino-N,N-dimethylbutyramide | HCID 136117660 | — |
| 溶媒 | Acetone | HCID 180 | — |
| 生成物 | 3-(4-methylbenzyloxyimino)-2-methoxyimino-N,N-dimethylbutyramide | HCID 53679960 | 96.5% |
反応手順
To a solution of 600 mg (3.2 mmol) of 3-hydroxyimino-2-methoxyimino-N,N-dimethylbutyramide in 20 ml of acetone, 500 mg (3.5 mmol) of 4-methylbenzylchloride and 660 mg (4.8 mmol) of potassium carbonate were added and the mixture was heated under reflux for 16 hours. The reaction mixture was combined with 30 ml of water and extracted three times with 30 ml of diethylether. After washing with water and a saturated aqueous sodium chloride, the mixture was dried over with anhydrous magnesium sulfate and then the solvent was distilled off. The residue thus obtained was purified by a column chromatography on a silica gel (n-hexane/ethyl acetate) to obtain 900 mg (yield: 96%) of 3-(4-methylbenzyloxyimino)-2-methoxyimino-N,N-dimethylbutyramide as a colorless crystal.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US06251949B1 |
|---|
| 出典データセット | uspto-grants-2001_06 |
|---|
| ORD ID | ord-4439910297a7458ab185eeef33af6f63 |
|---|
| 出典メモ | uspto-grants-2001_06 |
|---|