1,2-Ethanediamine, N1,N1-bis(1-methylethyl)- → HCID 23456456、化合物

HRID 1973461ノート

反応式

HRID 1973461 の反応式
[CH:1]([N:4]([CH2:8][CH2:9][NH2:10])[CH:5]([CH3:7])[CH3:6])([CH3:3])[CH3:2].[OH:11][C:12]1[CH:27]=[CH:26][C:15]([C:16](=O)[CH2:17][CH:18]2[CH2:23][CH2:22][CH2:21][CH2:20][C:19]2=O)=[CH:14][CH:13]=1>C(O)(=O)C.O.Cl>[CH:1]([N:4]([CH:5]([CH3:7])[CH3:6])[CH2:8][CH2:9][N:10]1[C:19]2[CH2:20][CH2:21][CH2:22][CH2:23][C:18]=2[CH:17]=[C:16]1[C:15]1[CH:14]=[CH:13][C:12]([OH:11])=[CH:27][CH:26]=1)([CH3:3])[CH3:2]

参加物

6

反応物 2

HCID 84591,2-Ethanediamine, N1,N1-bis(1-methylethyl)-HCID 12270333Cyclohexanone, 2-[2-(4-hydroxyphenyl)-2-oxoethyl]-

生成物 1

HCID 23456456HCID 23456456、化合物

試薬・触媒・溶媒 3

HCID 176Acetic Acid溶媒HCID 313Hydrochloric Acid溶媒HCID 962Water溶媒

実験手順

A solution of 5.77 g (0.04 mole) of diisopropylaminoethylamine and 9.3 g (0.04 mole) of 2-(p-hydroxyphenacyl) cyclohexanone in glacial acetic acid is refluxed under nitrogen for 14 hours, then cooled to ambient temperature and diluted with water and dilute hydrochloric acid. The aqueous solution is washed with ether, basified with 10% sodium carbonate and extracted with ether. After drying the ether solution over magnesium sulfate, the ether is removed to give a pale yellow solid. The solid is recrystallized from an ether-petroleum ether mixture to give pale yellow crystals of 1-(2-diisopropylaminoethyl)-2-(p-hydroxyphenyl)-4,5,6,7-tetrahydroindole as pale yellow crystals, m.p. 112°-114.5° C.

後処理

  1. washThe aqueous solution is washed with ether
  2. extractionextracted with ether
  3. dry with materialAfter drying the ether solution over magnesium sulfate
  4. customthe ether is removed
  5. customto give a pale yellow solid
  6. customThe solid is recrystallized from an ether-petroleum ether mixture

出典と根拠

ORDレコード
ord-6088b8d70ba448e280fdd279b831cbeb
出典データセット
uspto-grants-1976_12
特許番号
US03997557

反応ノート

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