Hydroxyamine hydrochloride → 4-Dimethylamino-1-methyl-4-phenyl-cyclohexane carbaldehyde oxime

HRID 76950ノート

反応式

HRID 76950 の反応式
[CH3:1][N:2]([CH3:18])[C:3]1([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:8][CH2:7][C:6]([CH3:11])([CH:9]=O)[CH2:5][CH2:4]1.Cl.[NH2:20][OH:21]>C(O)C>[CH3:1][N:2]([CH3:18])[C:3]1([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[CH2:8][CH2:7][C:6]([CH3:11])([CH:9]=[N:20][OH:21])[CH2:5][CH2:4]1

参加物

4

反応物 2

HCID 443297Hydroxyamine hydrochlorideHCID 866346824-Dimethylamino-1-methyl-4-phenyl-cyclohexane carbaldehyde

生成物 1

HCID 875238174-Dimethylamino-1-methyl-4-phenyl-cyclohexane carbaldehyde oxime

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of the title compound of step 2 (5.90 g, 24.0 mmol) and hydroxylamine hydrochloride (2.50 mg, 36.0 mmol) in abs. ethanol (100 mL) were mixed with Amberlyst A 21 (17.0 g) and stirred for 20 h at RT. The ion exchanger was filtered off, the solution concentrated to low volume and the residue made alkaline with 1N NaOH. The aqueous phase was extracted with ethyl acetate, dried over Na2SO4 and concentrated to low volume in a vacuum.

後処理

  1. filtrationThe ion exchanger was filtered off
  2. concentrationthe solution concentrated to low volume
  3. extractionThe aqueous phase was extracted with ethyl acetate
  4. dry with materialdried over Na2SO4
  5. concentrationconcentrated to low volume in a vacuum

出典と根拠

ORDレコード
ord-31acdb162e4348ad9fea701b1b6b1bc2
出典データセット
uspto-grants-2014_09
特許番号
US08835689B2

反応ノート

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