Dimethylamine → N,N,4-Trimethyl-5-nitropyridin-2-amine

HRID 1628505노트

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HRID 1628505 반응식
[CH3:1][NH:2][CH3:3].Cl[C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([N+:12]([O-:14])=[O:13])=[CH:7][N:6]=1>O1CCCC1>[CH3:1][N:2]([CH3:3])[C:5]1[CH:10]=[C:9]([CH3:11])[C:8]([N+:12]([O-:14])=[O:13])=[CH:7][N:6]=1

참가 물질

4

반응물 2

HCID 674DimethylamineHCID 3453642-Chloro-4-methyl-5-nitropyridine

생성물 1

HCID 21857174N,N,4-Trimethyl-5-nitropyridin-2-amine수율 99%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

Dimethylamine (50% solution in water, 20 mL) was added to a stirred solution of 2-chloro-4-methyl-5-nitropyridine (15.0 g, 86.9 mmol) in tetrahydrofuran (150 mL), and the mixture was stirred at 0° C. for 2 hr. The mixture was concentrated in vacuo, diluted with saturated aqueous sodium hydrogen carbonate and extracted with ethyl acetate. The combined organic layer was washed with brine, dried over anhydrous magnesium sulfate, filtered and concentrated in vacuo to give the title compound as a yellow solid (15.7 g, 86.6 mmol, 99%).

후처리

  1. concentrationThe mixture was concentrated in vacuo
  2. additiondiluted with saturated aqueous sodium hydrogen carbonate
  3. extractionextracted with ethyl acetate
  4. washThe combined organic layer was washed with brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo

출처 및 근거

ORD 기록
ord-10ff3fb2e3f64583826c6c984fb20f43
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08785460B2

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