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

HRID 1415546

반응식

HRID 1415546 반응식
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

참가 물질

4

반응물 2

HCID 125434549-AcetoxyxantheneHCID 214828091-Ethyl-3-methylaminopiperidine

생성물 1

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

시약·촉매·용매 1

HCID 241Benzene용매

실험 절차

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.

후처리

  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)

출처 및 근거

ORD 기록
ord-db5e2acb19934cfd9b687be4999bda80
출처 데이터셋
uspto-grants-1977_01
특허 번호
US04005208

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