m-Chloroperbenzoic acid → 1-Methyl-4-phenoxy-4-phenylpiperidine N-oxide

HRID 1156037노트

반응식

HRID 1156037 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][C:5]([O:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH2:4][CH2:3]1.ClC1C=CC=C(C(OO)=[O:29])C=1>CO>[CH3:1][N+:2]1([O-:29])[CH2:7][CH2:6][C:5]([O:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)([C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)[CH2:4][CH2:3]1

참가 물질

4

반응물 2

HCID 70297m-Chloroperbenzoic acidHCID 3060394Piperidine, 1-methyl-4-phenoxy-4-phenyl-

생성물 1

HCID 538883291-Methyl-4-phenoxy-4-phenylpiperidine N-oxide

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

1.5 g of 1-methyl-4-phenoxy-4-phenylpiperidine are dissolved in 4 ml of methanol, and 1.7 g of 80% strength m-chloroperbenzoic acid, dissolved in methanol, are added slowly thereto while cooling with ice. After stirring the mixture at room temperature for 3 hours, the solvent is stripped off and the residue is partitioned between concentrated sodium hydroxide solution and chloroform. The crude N-oxide hydrate (which remains after drying the chloroform phase and evaporating off the solvent) is taken up in a little methanol, and the equivalent amount of methanolic fumaric acid is added. 1 g of a colorless precipitate is obtained.

후처리

  1. additionare added slowly
  2. temperaturewhile cooling with ice
  3. customthe residue is partitioned between concentrated sodium hydroxide solution and chloroform
  4. dry with materialafter drying the chloroform phase
  5. customevaporating off the solvent)
  6. additionthe equivalent amount of methanolic fumaric acid is added

출처 및 근거

ORD 기록
ord-73c031d5a4e942119bc30554cd4ce55d
출처 데이터셋
uspto-grants-1982_06
특허 번호
US04333942

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