Sodium Hydroxide → HCID 13612399、化合物

HRID 441633

反応式

HRID 441633 の反応式
[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

参加物

6

反応物 3

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

生成物 1

HCID 13612399HCID 13612399、化合物

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d268194991154a7e9368e3ceae7d7c3e
出典データセット
uspto-grants-1977_08
特許番号
US04041165

関連ノート

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