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

HRID 1477210ノート

反応式

HRID 1477210 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-cf3794f8be844bfd9e09a54a4e9011a7
出典データセット
uspto-grants-2016_08
特許番号
US09403767B2

反応ノート

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