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Chloroform → 1-(2-Cyanoethylamino)-5-(4,6-dimethyl-2-pyrimidylamino)pentane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Chloroform | HCID 6212 | — |
| 反応物 | Acrylonitrile | HCID 7855 | — |
| 反応物 | 5-(4,6-Dimethyl-2-pyrimidylamino)-1-pentanamine | HCID 14346017 | — |
| 溶媒 | tert-Butanol | HCID 6386 | — |
| 生成物 | 1-(2-Cyanoethylamino)-5-(4,6-dimethyl-2-pyrimidylamino)pentane | HCID 14346018 | 85.8% |
反応手順
To a stirred solution of (XII) (966 mg) in t-butanol was added 250 mg of acrylonitrile dissolved in 1 ml t-butanol over a period of 1 hour. Continued stirring for 3.5 hours at room temperature and finally refluxed for 1.5 hours. Chloroform was added and the product was extracted into 1N H2SO4. The aqueous phase was washed once with CHCl3, then basified to pH 10 with 2N NaOH and the free amine extracted into CHCl3. The product (XIII) 1.04 g was obtained by evaporation of the solvents under vacuum.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04762949 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-910574ed73dc41d5b4fcb1ab0f5d4a28 |
| 出典メモ | uspto-grants-1988_08 |