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Citric Acid → 4-(3-Chloro-4-methoxybenzylamino)-5-methoxycarbonyl-6-(4-hydroxypiperidin-1-yl)-2-methylthiopyrimidine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Citric Acid | HCID 311 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Piperidin-4-ol | HCID 79341 | — |
| 反応物 | HCID 17848354 | HCID 17848354 | — |
| 溶媒 | Dimethylacetamide | HCID 31374 | — |
| 生成物 | 4-(3-Chloro-4-methoxybenzylamino)-5-methoxycarbonyl-6-(4-hydroxypiperidin-1-yl)-2-methylthiopyrimidine | HCID 17848321 | — |
反応手順
A mixture of 4-(3-chloro-4-methoxybenzylamino)-5-methoxycarbonyl-6-chloro-2-methylthiopyrimidine (prepared in the above (3)) 100 mg, 4-hydroxypiperidine 78 mg, triethylamine 0.11 ml and N,N-dimethylacetamide 3 ml is stirred at room temperature for 1 hour. The reaction mixture is diluted a 10% aqueous citric acid solution and extracted with ethyl acetate. The organic layer is washed, dried and concentrated in vacuo to give 4-(3-chloro-4-methoxybenzylamino)-5-methoxycarbonyl-6-(4-hydroxypiperidin-1-yl)-2-methylthiopyrimidine as a colorless caramel 132 mg.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07273868B2 |
| 出典データセット | uspto-grants-2007_09 |
| ORD ID | ord-19bca68de0704b2b8082decf0fda5bdb |
| 出典メモ | uspto-grants-2007_09 |