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Sodium Chloride → 3'-Chloroacetamidomethyl-4'-hydroxypropiophenone
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Sodium Chloride | HCID 5234 | — |
| 反応物 | 4'-Hydroxypropiophenone | HCID 6271 | — |
| 反応物 | N-Methylol-alpha-chloroacetamide | HCID 62466 | — |
| 溶媒 | Sulfuric Acid | HCID 1118 | — |
| 生成物 | 3'-Chloroacetamidomethyl-4'-hydroxypropiophenone | HCID 13631732 | 56.4% |
反応手順
To 40 ml of concentrated sulfuric acid with stirring under ice-cooling is added a mixture of 10 g of 4'-hydroxypropiophenone and 10 g of N-hydroxymethylchloroacetic amide in a small portion. After addition, the reaction mixture is further stirred under ice-cooling for 130 minutes. The resulting mixture is poured into ice-cold water containing sodium chloride and the solution is extracted with ethyl acetate. The ethyl acetate layer is washed with water and dried over sodium sulfate and then filtered. The filtrate is concentrated under reduced pressure and obtained white crystals are recrystallized from a mixture of hexane and ethanol to give 9.6 g of 3'-chloroacetamidomethyl-4'-hydroxypropiophenone as white crystals, melting at 143°-145° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04709095 |
| 出典データセット | uspto-grants-1987_11 |
| ORD ID | ord-632dcacfe34a41d6b24d0d2ec8ea2465 |
| 出典メモ | uspto-grants-1987_11 |