HCID 21419586, 화합물 → Bis(3-piperidinopropyl)fluorene-2,7-dicarboxylate dihydrochloride

HRID 1578640노트

반응식

HRID 1578640 반응식
[ClH:1].Cl.[N:3]1([CH2:9][CH2:10][CH2:11][O:12][C:13]([C:15]2[CH:27]=[CH:26][C:25]3[C:24]4[C:19](=[CH:20][C:21]([C:28]([O:30][CH2:31][CH2:32][CH2:33][N:34]5[CH2:39][CH2:38][CH2:37][CH2:36][CH2:35]5)=[O:29])=[CH:22][CH:23]=4)[C:18](=O)[C:17]=3[CH:16]=2)=[O:14])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1>O.[Pd]>[ClH:1].[ClH:1].[N:3]1([CH2:9][CH2:10][CH2:11][O:12][C:13]([C:15]2[CH:27]=[CH:26][C:25]3[C:24]4[C:19](=[CH:20][C:21]([C:28]([O:30][CH2:31][CH2:32][CH2:33][N:34]5[CH2:35][CH2:36][CH2:37][CH2:38][CH2:39]5)=[O:29])=[CH:22][CH:23]=4)[CH2:18][C:17]=3[CH:16]=2)=[O:14])[CH2:8][CH2:7][CH2:6][CH2:5][CH2:4]1

참가 물질

4

반응물 1

HCID 21419586HCID 21419586, 화합물

생성물 1

HCID 86733059Bis(3-piperidinopropyl)fluorene-2,7-dicarboxylate dihydrochloride

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 962Water용매

실험 절차

A solution of 20.0 g (0.04 mole) of bis(3-piperidinopropyl)-9-oxofluorene-2,7-dicarboxylate dihydrochloride in water to make a total volume of 240 ml is hydrogenated over 8.0 g of 10% palladium on charcoal for 2 days at 53°C on a Parr hydrogenation apparatus. The mixture is decanted from the catalyst, filtered through filter aid, treated with charcoal and refiltered. The solution is made basic to phenolphthalein with 20% sodium hydroxide and is extracted three times with CHCl3. The combined extracts are washed twice with water, dried over anhydrous sodium sulfate and filtered. The filtrate is made acidic to Congo Red with ethereal HCl. Most of the solvent is removed on a steam bath under vacuum, and the resulting solid is recrystallized from methanol-ether and from absolute ethanol and vacuum dried to give bis(3-piperidinopropyl)fluorene-2,7-dicarboxylate dihydrochloride.

후처리

  1. customThe mixture is decanted from the catalyst
  2. filtrationfiltered
  3. filtrationthrough filter aid
  4. additiontreated with charcoal
  5. extractionis extracted three times with CHCl3
  6. washThe combined extracts are washed twice with water
  7. dry with materialdried over anhydrous sodium sulfate
  8. filtrationfiltered
  9. customMost of the solvent is removed on a steam bath under vacuum
  10. customthe resulting solid is recrystallized from methanol-ether and from absolute ethanol and vacuum
  11. customdried

출처 및 근거

ORD 기록
ord-2dc1766a6e05424c8d12742bbaeb5c75
출처 데이터셋
uspto-grants-1976_02
특허 번호
US03937833

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