Ethanol → HCID 21419586, 화합물

HRID 1578639노트

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HRID 1578639 반응식
[CH:1]1[C:13]2[C:12](=[O:14])[C:11]3[C:6](=[CH:7][CH:8]=[C:9]([C:15]([Cl:17])=[O:16])[CH:10]=3)[C:5]=2[CH:4]=[CH:3][C:2]=1[C:18](Cl)=[O:19].[CH2:21]([OH:23])[CH3:22].[N:24]1([CH2:30][CH2:31][CH2:32][OH:33])[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1>C(Cl)(Cl)Cl>[ClH:17].[ClH:17].[N:24]1([CH2:30][CH2:22][CH2:21][O:23][C:18]([C:2]2[CH:3]=[CH:4][C:5]3[C:6]4[C:11](=[CH:10][C:9]([C:15]([O:33][CH2:32][CH2:31][CH2:30][N:24]5[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]5)=[O:16])=[CH:8][CH:7]=4)[C:12](=[O:14])[C:13]=3[CH:1]=2)=[O:19])[CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1

참가 물질

5

반응물 3

HCID 702EthanolHCID 66032Piperidine-1-propanolHCID 214196159-Oxo-fluorene-2,7-dicarbonyl chloride

생성물 1

HCID 21419586HCID 21419586, 화합물

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

A suspension of 30.5 g (0.12 mole) of fluoren-9-one-2,7-dicarbonyl chloride in 1 liter of dry chloroform free from ethanol is stirred and treated with 37.5 g (0.26 mole) of 3-piperidino-1-propanol resulting in a mildly exothermic reaction. The resulting mixture is stirred and refluxed for two hours, cooled to room temperature, filtered, and the filtrate washed three times with 250 ml portions of saturated sodium bicarbonate solution. The chloroform solution is then washed with water and saturated sodium chloride solution, dried over anhydrous sodium sulfate, and filtered. Most of the solvent is removed from the filtrate on a steam bath under vacuum, and the residue is dissolved in butanone. The solution is made acidic to Congo Red with ethereal HCl causing the product to precipitate as a yellow crystalline solid. The solid is filtered, recrystallized from butanone-methanol and dried to give bis(3-piperidinopropyl)-9-oxofluorene-2,7-dicarboxylate dihydrochloride, M.P. 2.93°-295°C (dec.).

후처리

  1. stirringThe resulting mixture is stirred
  2. temperaturerefluxed for two hours
  3. filtrationfiltered
  4. washthe filtrate washed three times with 250 ml portions of saturated sodium bicarbonate solution
  5. washThe chloroform solution is then washed with water and saturated sodium chloride solution
  6. dry with materialdried over anhydrous sodium sulfate
  7. filtrationfiltered
  8. customMost of the solvent is removed from the filtrate on a steam bath under vacuum
  9. dissolutionthe residue is dissolved in butanone
  10. customto precipitate as a yellow crystalline solid
  11. filtrationThe solid is filtered
  12. customrecrystallized from butanone-methanol
  13. customdried

출처 및 근거

ORD 기록
ord-1eee7b0e6168456890cad10dc0a6c6a5
출처 데이터셋
uspto-grants-1976_02
특허 번호
US03937833

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