9-Acetoxyxanthene → N-methyl-N-(N-ethyl-3-piperidinyl)-9-xanthenylamine

HRID 1415546

反応式

HRID 1415546 の反応式
C(O[CH:5]1[C:18]2[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=2[O:12][C:11]2[C:6]1=[CH:7][CH:8]=[CH:9][CH:10]=2)(=O)C.[CH2:19]([N:21]1[CH2:26][CH2:25][CH2:24][CH:23]([NH:27][CH3:28])[CH2:22]1)[CH3:20]>C1C=CC=CC=1>[CH3:28][N:27]([CH:5]1[C:6]2[CH:7]=[CH:8][CH:9]=[CH:10][C:11]=2[O:12][C:13]2[C:18]1=[CH:17][CH:16]=[CH:15][CH:14]=2)[CH:23]1[CH2:24][CH2:25][CH2:26][N:21]([CH2:19][CH3:20])[CH2:22]1

参加物

4

反応物 2

HCID 125434549-AcetoxyxantheneHCID 214828091-Ethyl-3-methylaminopiperidine

生成物 1

HCID 21482827N-methyl-N-(N-ethyl-3-piperidinyl)-9-xanthenylamine

試薬・触媒・溶媒 1

HCID 241Benzene溶媒

実験手順

A solution of 3.7 g. (15.4 mmoles) of 9-acetoxyxanthene and 2.2 g. (15.5 mmoles) of 1-ethyl-3-methylaminopiperidine in 80 ml. of benzene was refluxed under nitrogen for 22.5 hours. It was then cooled to room temperature, washed with aqueous sodium bicarbonate solution, and dried over potassium carbonate. After removal of solvent in vacuo, the residue was dissolved in 25 ml. of petroleum ether and filtered from a small amount of crystals. The filtrate was then concentrated in vacuo and chromatographed on silica gel (ether solvent) to give N-methyl-N-(N-ethyl-3-piperidinyl)-9-xanthenylamine.

後処理

  1. washwashed with aqueous sodium bicarbonate solution
  2. dry with materialdried over potassium carbonate
  3. customAfter removal of solvent in vacuo
  4. dissolutionthe residue was dissolved in 25 ml
  5. filtrationof petroleum ether and filtered from a small amount of crystals
  6. concentrationThe filtrate was then concentrated in vacuo
  7. customchromatographed on silica gel (ether solvent)

出典と根拠

ORDレコード
ord-db5e2acb19934cfd9b687be4999bda80
出典データセット
uspto-grants-1977_01
特許番号
US04005208

関連ノート

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