反応式
[CH3:1][N:2]([CH3:11])[CH2:3][CH2:4][CH:5]1[CH2:10][CH2:9][CH2:8][CH2:7][NH:6]1.C(O[CH:16]1[C:29]2[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=2[O:23][C:22]2[C:17]1=[CH:18][CH:19]=[CH:20][CH:21]=2)(=O)C>C1C=CC=CC=1>[CH:18]1[C:17]2[CH:16]([N:6]3[CH2:7][CH2:8][CH2:9][CH2:10][CH:5]3[CH2:4][CH2:3][N:2]([CH3:1])[CH3:11])[C:29]3[C:24](=[CH:25][CH:26]=[CH:27][CH:28]=3)[O:23][C:22]=2[CH:21]=[CH:20][CH:19]=1参加物
4
実験手順
A solution of 3.12 g. (0.02 mole) of 2-(2-dimethylaminoethyl)piperidine and 4.8 g. (0.02 mole) of 9-acetoxyxanthene in 75 ml. of anhydrous benzene was refluxed for 20 hours. The cooled solution was washed with 100 ml. of a 5 percent aqueous sodium bicarbonate solution, dried over anhydrous potassium carbonate, filtered, and evaporated in vacuo. The residue was taken up in low boiling petroleum ether and filtered to remove dixanthenyl ether. The filtrate was chromatographed on 125 g. of alumina, eluting successively with petroleum ether, petroleum etherbenzene mixtures, benzene, and finally ether. Evaporation of the ether fractions gave 1-(9-xanthenyl)-2-(2-dimethylaminoethyl)piperidine, m.p. 64°-67°C.
後処理
- washThe cooled solution was washed with 100 ml
- dry with materialof a 5 percent aqueous sodium bicarbonate solution, dried over anhydrous potassium carbonate
- filtrationfiltered
- customevaporated in vacuo
- filtrationfiltered
- customto remove dixanthenyl ether
- customThe filtrate was chromatographed on 125 g
- washof alumina, eluting successively with petroleum ether, petroleum etherbenzene mixtures, benzene, and finally ether
- customEvaporation of the ether fractions
出典と根拠
- ORDレコード
- ord-613d4b6d8ccd46bf882576d6fb7b57c2
- 出典データセット
- uspto-grants-1976_09
- 特許番号
- US03980788
関連ノート
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