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

HRID 1156037

反応式

HRID 1156037 の反応式
[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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒2 回

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-73c031d5a4e942119bc30554cd4ce55d
出典データセット
uspto-grants-1982_06
特許番号
US04333942

関連ノート

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