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

HRID 1576965노트

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HRID 1576965 반응식
[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

참가 물질

6

반응물 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

생성물 1

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

시약·촉매·용매 1

HCID 962Water용매

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온도
80 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-50733dc07a8d4fe88d0b5fb3faa15cab
출처 데이터셋
uspto-grants-1976_09
특허 번호
US03983124

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