Methyl iodide → 4-Dimethylamino-1-methyl-4-phenyl-cyclohexane carbaldehyde

HRID 1477209노트

반응식

HRID 1477209 반응식
[CH3:1][N:2]([CH3:17])[C:3]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:8][CH2:7][CH:6]([CH:9]=[O:10])[CH2:5][CH2:4]1.[C:18](O[K])(C)(C)C.CI>ClCCl>[CH3:1][N:2]([CH3:17])[C:3]1([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH2:8][CH2:7][C:6]([CH3:18])([CH:9]=[O:10])[CH2:5][CH2:4]1

참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 104439064-Dimethylamino-4-phenylcyclohexanecarbaldehydeHCID 178418922HCID 178418922, 화합물

생성물 1

HCID 866346824-Dimethylamino-1-methyl-4-phenyl-cyclohexane carbaldehyde

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of the title compound from step 1 (11.6 g, 50.0 mmol) in abs. dichloromethane (200 mL) was mixed with tert-BuOK (6.50 g, 58.0 mmol) and methyl iodide (3.42 mL, 55.0 mmol) at 0° C. in argon. After 30 min the batch was heated to RT and then stirred overnight (solid separated out). The reaction mixture was washed with water and saturated NaCl solution (50 mL), dried over Na2SO4, concentrated to low volume in a vacuum and the remaining residue purified by flash chromatography with ethyl acetate/MeOH 20:1.

후처리

  1. custom(solid separated out)
  2. washThe reaction mixture was washed with water and saturated NaCl solution (50 mL)
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated to low volume in a vacuum
  5. customthe remaining residue purified by flash chromatography with ethyl acetate/MeOH 20:1

출처 및 근거

ORD 기록
ord-d007b93799a44017a471782931aed507
출처 데이터셋
uspto-grants-2016_08
특허 번호
US09403767B2

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