関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | 1-Methylpiperazine | HCID 53167 | — |
| 反応物 | 3-Chloropropyl (3-hydroxymethylphenyl)carbamate | HCID 59564725 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | 3-(4-Methylpiperazin-1-yl)propyl (3-hydroxymethylphenyl)carbamate | HCID 59564727 | — |
反応手順
10 g (100 mmol) of N-methylpiperazine are added to a solution of 2.4 g (10 mmol) of 3-chloropropyl (3-hydroxymethylphenyl)carbamate in 10 ml of acetonitrile. The solution is refluxed for 4 h. The mixture is then hydrolysed by addition of water and cooled to about 65° C., and ethyl acetate is added. The mixture is then cooled to room temperature, during which the product is obtained as a solid between the organic and aqueous phases. The product is filtered off and rinsed with water, acetonitrile and ethyl acetate. The product is subsequently dried at 50° C. for several hours; ESI: 308 (M+H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08431572B2 |
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| 出典データセット | uspto-grants-2013_04 |
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| ORD ID | ord-ed3e98c6235c491e92708a170981fb1e |
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| 出典メモ | uspto-grants-2013_04 |
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