HCID 21419586、化合物 → Bis(3-piperidinopropyl)fluorene-2,7-dicarboxylate dihydrochloride

HRID 1578640ノート

反応式

HRID 1578640 の反応式
[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

参加物

4

反応物 1

HCID 21419586HCID 21419586、化合物

生成物 1

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

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-2dc1766a6e05424c8d12742bbaeb5c75
出典データセット
uspto-grants-1976_02
特許番号
US03937833

反応ノート

読み込み中…