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Acetic Acid → 1-Methyl-6-(N-chloroacetylaminomethyl)-5-indanol
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | N-Methylol-alpha-chloroacetamide | HCID 62466 | — |
| 反応物 | 1-Methylindan-5-ol | HCID 89312 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-Methyl-6-(N-chloroacetylaminomethyl)-5-indanol | HCID 20287720 | — |
反応手順
A solution of 850 mg of 1 methyl-5-indanol in 5 ml of a mixed solution of acetic acid and sulfuric acid (10:1 by volume) solution was mixed with 850 mg of N-hydroxymethyl chloroacetamide at room temperature under stirring for 2 hours. After reaction the reaction mixture was poured into 20 ml of water, extracted with ethyl acetate. The extract was washed with water, dried with anhydrous magnesium sulfate and concentrated under vacuum. The crude product thus obtained was purified by column chromatography on 100 g of Kiesel gel using an eluting agent comprising a mixture (20:1 by volume) of methylene chloride and ethyl acetate to provide 590 mg of the titled compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04254056 |
| 出典データセット | uspto-grants-1981_03 |
| ORD ID | ord-355a568de3424f56a7233b33c105c578 |
| 出典メモ | uspto-grants-1981_03 |