Piperidine, 1-(3-chloropropyl)- → Bis(3-piperidinopropyl) 9-ethylcarbazole-3,6-dicarboxylate dihydrochloride

HRID 441630

반응식

HRID 441630 반응식
[CH2:1]([N:3]1[C:15]2[CH:14]=[CH:13][C:12]([C:16]([OH:18])=[O:17])=[CH:11][C:10]=2[C:9]2[C:4]1=[CH:5][CH:6]=[C:7]([C:19]([OH:21])=[O:20])[CH:8]=2)[CH3:2].[N:22]1([CH2:28][CH2:29][CH2:30][Cl:31])[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1>[Cl-].C([N+](C)(C)C)C1C=CC=CC=1.C(O)(C)C>[ClH:31].[ClH:31].[N:22]1([CH2:28][CH2:29][CH2:30][O:20][C:19]([C:7]2[CH:6]=[CH:5][C:4]3[N:3]([CH2:1][CH3:2])[C:15]4[C:10]([C:9]=3[CH:8]=2)=[CH:11][C:12]([C:16]([O:18][CH2:30][CH2:29][CH2:28][N:22]2[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]2)=[O:17])=[CH:13][CH:14]=4)=[O:21])[CH2:27][CH2:26][CH2:25][CH2:24][CH2:23]1

참가 물질

5

반응물 2

HCID 79625Piperidine, 1-(3-chloropropyl)-HCID 37979149-ethyl-9H-carbazole-3,6-dicarboxylic acid

생성물 1

HCID 21419565Bis(3-piperidinopropyl) 9-ethylcarbazole-3,6-dicarboxylate dihydrochloride

시약·촉매·용매 2

HCID 5963Benzyltrimethylammonium chloride촉매HCID 3776Isopropanol용매

실험 절차

To 250 ml of isopropyl alcohol is added one equivalent of 9-ethylcarbazole-3,6-dicarboxylic acid, 2 equivalents of 3-piperidinopropylchloride, and a catalytic amount of benzyltrimethylammonium chloride. The mixture is heated to reflux for 2 hours. Upon cooling a solid forms which is collected, washed with ether, dried and dissolved in water. The aqueous solution is made basic with saturated sodium bicarbonate, and the product is extracted with ether. The ether solution is washed with water, dried, and acidified with ethereal HCl. The resulting precipitate is recrystallized from methanol-butanone to give bis(3-piperidinopropyl)-9-ethylcarbazole-3,6-dicarboxylate dihydrochloride.

후처리

  1. temperatureThe mixture is heated
  2. temperatureto reflux for 2 hours
  3. temperatureUpon cooling a solid forms which
  4. customis collected
  5. washwashed with ether
  6. customdried
  7. dissolutiondissolved in water
  8. extractionthe product is extracted with ether
  9. washThe ether solution is washed with water
  10. customdried
  11. customThe resulting precipitate is recrystallized from methanol-butanone

출처 및 근거

ORD 기록
ord-911df8559773457783bef87d2651d22c
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04041165

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