関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Iodide | HCID 4875 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 2-Chloro-N-(2,6-dimethylphenyl)acetamide | HCID 70798 | — |
| 反応物 | alpha-Methyl-4-(phenylmethyl)-2-piperazinemethanol | HCID 14230267 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | N-(2,6-dimethylphenyl)-2-(1-hydroxyethyl)-4-(phenylmethyl)-1-piperazineacetamide | HCID 14230222 | 84.8% |
反応手順
A mixture of 24.0 parts of α-methyl-4-(phenylmethyl)-2-piperazinemethanol, 27.3 parts of 2-chloro-N-(2,6-dimethylphenyl)acetamide, 25.4 parts of sodium carbonate, 0.1 parts of potassium iodide and 180 parts of N,N-dimethylformamide was stirred for 18 hours at 60° C. The reaction mixture was poured onto water and the product was extracted with dichloromethane. The extract was washed with water, dried, filtered and evaporated. The residue was purified by column-chromatography over silica gel using a mixture of trichloromethane and methanol (90:10 by volume) as eluent. The pure fractions were collected and the eluent was evaporated. The residue was crystallized from 1,1'-oxybisethane, yielding 35.19 parts (84.8%) of N-(2,6-dimethylphenyl)-2-(1-hydroxyethyl)-4-(phenylmethyl)-1-piperazineacetamide; mp. 148.8° C. (compound 113).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04766125 |
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| 出典データセット | uspto-grants-1988_08 |
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| ORD ID | ord-75fdca07dd8d42d88dc2c02046d78d62 |
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| 出典メモ | uspto-grants-1988_08 |
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