Dimethyl-(2-piperidin-2-yl-ethyl)-amine → 1-(9-Xanthenyl)-2-(2-dimethylaminoethyl)piperidine

HRID 1576393

반응식

HRID 1576393 반응식
[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

참가 물질

4

반응물 2

HCID 296295Dimethyl-(2-piperidin-2-yl-ethyl)-amineHCID 125434549-Acetoxyxanthene

생성물 1

HCID 215125501-(9-Xanthenyl)-2-(2-dimethylaminoethyl)piperidine

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  1. washThe cooled solution was washed with 100 ml
  2. dry with materialof a 5 percent aqueous sodium bicarbonate solution, dried over anhydrous potassium carbonate
  3. filtrationfiltered
  4. customevaporated in vacuo
  5. filtrationfiltered
  6. customto remove dixanthenyl ether
  7. customThe filtrate was chromatographed on 125 g
  8. washof alumina, eluting successively with petroleum ether, petroleum etherbenzene mixtures, benzene, and finally ether
  9. customEvaporation of the ether fractions

출처 및 근거

ORD 기록
ord-613d4b6d8ccd46bf882576d6fb7b57c2
출처 데이터셋
uspto-grants-1976_09
특허 번호
US03980788

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