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

HRID 1477210노트

반응식

HRID 1477210 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-cf3794f8be844bfd9e09a54a4e9011a7
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09403767B2

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