Sodium Hydroxide → HCID 13612399, 화합물

HRID 441633

반응식

HRID 441633 반응식
[OH:1][C:2]1[CH:14]=[CH:13][C:12]2[C:11]3[C:6](=[CH:7][C:8]([OH:15])=[CH:9][CH:10]=3)[C:5](=[O:16])[C:4]=2[CH:3]=1.[ClH:17].[N:18]1([CH2:24][CH2:25][Cl:26])[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1.[OH-].[Na+]>C1(C)C=CC=CC=1.O>[ClH:26].[ClH:17].[N:18]1([CH2:24][CH2:25][O:1][C:2]2[CH:14]=[CH:13][C:12]3[C:11]4[C:6](=[CH:7][C:8]([O:15][CH2:25][CH2:24][N:18]5[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]5)=[CH:9][CH:10]=4)[C:5](=[O:16])[C:4]=3[CH:3]=2)[CH2:23][CH2:22][CH2:21][CH2:20][CH2:19]1

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 74826Piperidine, 1-(2-chloroethyl)-, hydrochlorideHCID 43541812,7-Dihydroxyfluoren-9-one

생성물 1

HCID 13612399HCID 13612399, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 1140Toluene용매

실험 절차

A mixture of 5.3 g (0.025 mole) of 2,7-dihydroxyfluoren-9-one in 100 ml of toluene, 16.2 g (0.088 mole) of 2-piperidinoethylchloride hydrochloride and 5.0 g (0.125 mole) of sodium hydroxide in 40 ml of water is heated at reflux for 15 hours with stirring. Upon cooling, the layers are separated. The toluene layer is washed with water and saturated sodium chloride solution, dried over anhydrous magnesium sulfate and filtered. The filtrate is acidified to Congo Red with ethereal HCl, and the resulting precipitate is collected, washed with ether and recrystallized from butanone-methanol to give 2,7-bis(2-piperidinoethoxy)fluoren-9-one dihydrochloride, M.P. 304°-306° C.

후처리

  1. temperatureis heated
  2. temperatureat reflux for 15 hours
  3. temperatureUpon cooling
  4. customthe layers are separated
  5. washThe toluene layer is washed with water and saturated sodium chloride solution
  6. dry with materialdried over anhydrous magnesium sulfate
  7. filtrationfiltered
  8. customthe resulting precipitate is collected
  9. washwashed with ether
  10. customrecrystallized from butanone-methanol

출처 및 근거

ORD 기록
ord-d268194991154a7e9368e3ceae7d7c3e
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04041165

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