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Hydrochloric Acid → [(2,4-Dimethoxyphenyl)methyl](methyl)amine

HRID 1426695
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HRID 1426695 반응식
[CH3:1][O:2][C:3]1[CH:10]=[C:9]([O:11][CH3:12])[CH:8]=[CH:7][C:4]=1[CH:5]=O.[CH3:13][NH2:14].[BH4-].[Na+].Cl>CO>[CH3:1][O:2][C:3]1[CH:10]=[C:9]([O:11][CH3:12])[CH:8]=[CH:7][C:4]=1[CH2:5][NH:14][CH3:13]
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참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 6329MethylamineHCID 691752,4-DimethoxybenzaldehydeHCID 4311764Sodium borohydride

생성물 1

HCID 2416536[(2,4-Dimethoxyphenyl)methyl](methyl)amine수율 81%

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

2,4-Dimethoxybenzaldehyde (5.0 g) was dissolved in methanol (60 mL), and a 40% methanol solution (9.3 mL) of methylamine was added at room temperature. The mixture was stirred at room temperature for 1 hr, and sodium borohydride (1.37 g) was added by small portions under ice-cooling. The mixture was stirred at room temperature for 3 hr, treated with 1 mol/L hydrochloric acid under ice-cooling, and methanol was evaporated under reduced pressure. The residue was diluted with ethyl acetate, basified with saturated aqueous sodium hydrogen carbonate solution, and extracted with ethyl acetate. The extract was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was purified by basic silica gel column chromatography (eluent: hexane:ethyl acetate=4:1→2:1) to give the title compound as a colorless oil (yield 4.41 g, 81%).

후처리

  1. temperaturecooling
  2. stirringThe mixture was stirred at room temperature for 3 hr
  3. temperaturecooling
  4. custommethanol was evaporated under reduced pressure
  5. additionThe residue was diluted with ethyl acetate
  6. extractionextracted with ethyl acetate
  7. washThe extract was washed with saturated brine
  8. dry with materialdried over anhydrous sodium sulfate
  9. concentrationconcentrated under reduced pressure
  10. customThe residue was purified by basic silica gel column chromatography (eluent: hexane:ethyl acetate=4:1→2:1)

출처 및 근거

ORD 기록
ord-ebcde0bc413b4de382768e90dc2c129d
출처 데이터셋
uspto-grants-2015_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08933105B2

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