Hydrochloric Acid → 2,7-Bis(4-piperidino-1-buten-1-yl)fluorene

HRID 1576965ノート

反応式

HRID 1576965 の反応式
[N:1]1([CH2:7][CH2:8][CH2:9][CH:10]([C:12]2[CH:24]=[CH:23][C:22]3[C:21]4[C:16](=[CH:17][C:18]([CH:25]([CH2:27][CH2:28][CH2:29][N:30]5[CH2:35][CH2:34][CH2:33][CH2:32][CH2:31]5)O)=[CH:19][CH:20]=4)[CH2:15][C:14]=3[CH:13]=2)O)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1.Cl.C(OCCO)C.[OH-].[Na+]>O>[N:1]1([CH2:7][CH2:8][CH:9]=[CH:10][C:12]2[CH:24]=[CH:23][C:22]3[C:21]4[C:16](=[CH:17][C:18]([CH:25]=[CH:27][CH2:28][CH2:29][N:30]5[CH2:31][CH2:32][CH2:33][CH2:34][CH2:35]5)=[CH:19][CH:20]=4)[CH2:15][C:14]=3[CH:13]=2)[CH2:6][CH2:5][CH2:4][CH2:3][CH2:2]1

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 8076Glycol monoethyl etherHCID 14798Sodium HydroxideHCID 5153251-[7-[1-hydroxy-4-(1-piperidyl)butyl]-9H-fluoren-2-yl]-4-(1-piperidyl)butan-1-ol

生成物 1

HCID 541362442,7-Bis(4-piperidino-1-buten-1-yl)fluorene

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
80 °C

実験手順

A mixture of 4.7 g (0.01 mole) of α,α'-bis(3-piperidinopropyl)-2,7-fluorenedimethanol, 25 ml of concentrated hydrochloric acid and 25 ml of ethylene glycol monoethyl ether is heated at 80°C. for 5 minutes. The solution is diluted with water, made alkaline with a 20% sodium hydroxide solution and the solution is extracted with ether. The ether extract is washed with water, dried over magnesium sulfate and evaporated in vacuo. The residue is crystallized from isopropanol resulting in the preparation of crystalline 2,7-bis(4-piperidino-1-buten-1-yl)fluorene.

後処理

  1. extractionthe solution is extracted with ether
  2. extractionThe ether extract
  3. washis washed with water
  4. dry with materialdried over magnesium sulfate
  5. customevaporated in vacuo
  6. customThe residue is crystallized from isopropanol resulting in the preparation of crystalline 2,7-bis(4-piperidino-1-buten-1-yl)fluorene

出典と根拠

ORDレコード
ord-50733dc07a8d4fe88d0b5fb3faa15cab
出典データセット
uspto-grants-1976_09
特許番号
US03983124

反応ノート

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