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Methyl iodide → HCID 87523600, 화합물

HRID 1477196
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HRID 1477196 반응식
[CH3:1][N:2]([CH3:18])[C:3]1([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[CH:12]=2)[CH2:8][CH2:7][CH:6]([CH:9]=[O:10])[CH2:5][CH2:4]1.[C:19](O[K])(C)(C)C.CI>ClCCl>[CH3:1][N:2]([CH3:18])[C:3]1([C:11]2[CH:16]=[CH:15][CH:14]=[C:13]([F:17])[CH:12]=2)[CH2:8][CH2:7][C:6]([CH3:19])([CH:9]=[O:10])[CH2:5][CH2:4]1
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참가 물질

5

반응물 3

HCID 6328Methyl iodideHCID 866346814-Dimethylamino-4-(3-fluorophenyl)cyclohexanecarbaldehydeHCID 178418922HCID 178418922, 화합물

생성물 1

HCID 87523600HCID 87523600, 화합물

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

A solution of the title compound of step 1 (2.73 g, 10.95 mmol) in abs. dichloromethane (50 mL) was mixed with tert-BuOK (1.47 g, 13.14 mmol) and methyl iodide (747 μl, 12 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 mixed with saturated NaCl solution (50 mL) and extracted with dichloromethane (3×30 mL). The combined organic phases were dried over Na2SO4, concentrated to low volume in a vacuum and the remaining residue was purified by flash chromatography with ethyl acetate/MeOH 20:1.

후처리

  1. custom(solid separated out)
  2. additionThe reaction mixture was mixed with saturated NaCl solution (50 mL)
  3. extractionextracted with dichloromethane (3×30 mL)
  4. dry with materialThe combined organic phases were dried over Na2SO4
  5. concentrationconcentrated to low volume in a vacuum
  6. customthe remaining residue was purified by flash chromatography with ethyl acetate/MeOH 20:1

출처 및 근거

ORD 기록
ord-0da8bb2b40724bed91180d189ab66977
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09403767B2

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