関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetamide | HCID 178 | — |
| 反応物 | Pyridine | HCID 1049 | — |
| 反応物 | Dichloromethane | HCID 6344 | — |
| 反応物 | (19S)-5,19-diethyl-19-hydroxy-17-oxa-3,13-diazapentacyclo[11.8.0.02,11.04,9.015,20]henicosa-1(21),2(11),4,6,9,15(20)-hexaene-8,14,18-trione | HCID 178436639 | — |
| 溶媒 | Triethylamine | HCID 8471 | — |
| 生成物 | 4-Piperidinopiperidine-1-carbonyl chloride | HCID 9813375 | — |
反応手順
In a suitable vessel were charged 7-Ethyl-10-hydroxycamptothecin (20 g), methylene dichloride, acetamide (3 gm) and pyridine (60 ml) under nitrogen atmosphere. A solution of [1,4′]bipiperidinyl-1′-carbonyl chloride (17.6 g), methylene dichloride and triethylamine (20 ml) was prepared and added to the above suspension and stirred at 30-40° C. for 2 hours. The solvent was distilled out under reduced pressure at 50° C. and hexane was added under stirring as an antisolvent to isolate crystalline compound. The crystalline compound was filtered, washed with hexane and dried under reduced pressure at 50° C. The yield was 28.4 g (95%). HPLC Purity—99.9%
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US08546573B2 |
|---|
| 出典データセット | uspto-grants-2013_10 |
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| ORD ID | ord-6518246a8d4847cfa3c153f2d56092e4 |
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| 出典メモ | uspto-grants-2013_10 |
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