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Acetamide → 3,5-Dihydroxy-4-phenylazo-benzoic acid methyl ester
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetamide | HCID 178 | — |
| 反応物 | Bromine | HCID 24408 | — |
| 反応物 | Bromosuccinimide | HCID 38309 | — |
| 反応物 | 3-Hydroxy-5-keto-4-phenylazo-3-cyclohexenecarboxylic acid methyl ester | HCID 136056374 | — |
| 溶媒 | Chloroform | HCID 6212 | — |
| 生成物 | 3,5-Dihydroxy-4-phenylazo-benzoic acid methyl ester | HCID 136059786 | — |
反応手順
54.8 G. of 3-hydroxy-5-keto-4-phenylazo-3-cyclohexene-carboxylic acid methyl ester, 12.0 g. of acetamide and 2.0 g. of bromosuccinimide were stirred in 600 ml. of chloroform and treated dropwise with 32.0 g. of bromine in 400 ml. of chloroform (the reaction temperature being held below 35° C.). Soon, the separation of acetamide hydrobromide began. The mixture was stirred for an additional 30 minutes at room temperature. Then, the acetamide hydrobromide was removed by filtration and the filtrate evaporated to dryness. The residue was taken up in a small amount of ethanol, filtered under vacuum and washed with ethanol, whereby there was obtained 3,5-dihydroxy-4-phenylazo-benzoic acid methyl ester having a melting point of 216°-218° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04515948 |
| 出典データセット | uspto-grants-1985_05 |
| ORD ID | ord-3a63bdba080c4d18801dfb1b5fefe2a2 |
| 出典メモ | uspto-grants-1985_05 |