関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Chlorambucil | HCID 2708 | — |
| 反応物 | Prednisolone | HCID 5755 | — |
| 反応物 | p-Toluenesulfonic acid | HCID 6101 | — |
| 反応物 | Dicyclohexylcarbodiimide | HCID 10868 | — |
| 触媒 | 4-(Dimethylamino)pyridine | HCID 14284 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | Prednimustine | HCID 34457 | 91% |
反応手順
To 250 ml CH2Cl2 is added with stirring 36 g prednisolone (0.10 mol), 31.3 g chlorambucil (0,103 mol), 1.2 g DMAP (0,01 mol) and 1.1 g pTSA (0,06 mol). The reaction mixture is cooled to 0° C. and with continued stirring at this temperature a solution of 22.7 g DCC (0,11 mol) in 50 ml CH2Cl2 is slowly added. The reaction mixture is then kept at 0° C. with stirring for 20 h. 3 ml acetic acid is added and precipitated urea filtered off. The filtrate is evaporated in vacuo and the residue recrystallized from ethanol to give 58.9 g of TLC pure prednimustine (91% yield) without any discolouration. M.P. 165°-166° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US04537722 |
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| 出典データセット | uspto-grants-1985_08 |
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| ORD ID | ord-55fd81bfd4974c2a87c86e5c323af55e |
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| 出典メモ | uspto-grants-1985_08 |
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