反応式
CCC1C=CC(=O)[C:5]2=C[C:7]3[CH2:25][N:24]4[C:10](=[CH:11][C:12]5[C@@](O)(CC)C(=O)OC[C:13]=5[C:22]4=O)[C:8]=3[NH:9][C:4]=12.[CH2:30]([Cl:32])Cl.CN(C)C=[O:36].N1C=CC=CC=1>C(N(CC)CC)C>[N:24]1([CH:25]2[CH2:5][CH2:4][N:9]([C:30]([Cl:32])=[O:36])[CH2:8][CH2:7]2)[CH2:22][CH2:13][CH2:12][CH2:11][CH2:10]1参加物
6
反応物 4
生成物 1
試薬・触媒・溶媒 1
反応条件
- 温度
- 35 °C
実験手順
In a suitable vessel were charged 7-Ethyl-10-hydroxycamptothecin (1 g), methylene dichloride, dimethylformamide (0.186 gm) and pyridine (3 ml) under nitrogen atmosphere. A solution of [1,4′]bipiperidinyl-1′-carbonyl chloride (0.88 g), methylene dichloride and triethylamine (1 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, which was then filtered, washed with hexane and dried under reduced pressure at 50° C. The yield was 1.30 g (86.89%); HPLC purity—99.8%
後処理
- additionadded to the above suspension
- distillationThe solvent was distilled out under reduced pressure at 50° C.
- additionhexane was added
- stirringunder stirring as an antisolvent
- customto isolate crystalline compound, which
- filtrationwas then filtered
- washwashed with hexane
- customdried under reduced pressure at 50° C
出典と根拠
- ORDレコード
- ord-dad8ff0cac2948c4b0cd6eb100d618d6
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08546573B2
関連ノート
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