Methylamine → N2,6-Dimethylpyridine-2,3-diamine

HRID 2220071노트

반응식

HRID 2220071 반응식
Cl[C:2]1[C:7]([N+:8]([O-])=O)=[CH:6][CH:5]=[C:4]([CH3:11])[N:3]=1.[CH3:12][NH2:13].[H][H]>CO.[Pd]>[CH3:11][C:4]1[N:3]=[C:2]([NH:13][CH3:12])[C:7]([NH2:8])=[CH:6][CH:5]=1

참가 물질

6

반응물 3

HCID 6329MethylamineHCID 12682302-Chloro-6-methyl-3-nitropyridineHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 22036951N2,6-Dimethylpyridine-2,3-diamine수율 83%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매2회

실험 절차

2-Chloro-6-methyl-3-nitropyridine (2.5 g, 14.5 mmol) was stirred in 1.0 M solution of methylamine (40 ml, 40 mmol) in methanol at 70° C. for 60 min. After cooling to ambient temperature, and methanol (60 ml) and 10% palladium on activated carbon were added and the resulting mixture was shaken under 40 psi of hydrogen gas at ambient temperature for 30 min. The mixture was filtered through a pad of Celite and concentrated in vacuum. Chromatography on silica gel, eluting with a mixture dichloromethane-methanol-38% aqueous ammonia (9:1:0.1) yielded the title compound (1.65 g, 83%).

후처리

  1. filtrationThe mixture was filtered through a pad of Celite
  2. concentrationconcentrated in vacuum
  3. washChromatography on silica gel, eluting with a mixture dichloromethane-methanol-38% aqueous ammonia (9:1:0.1)

출처 및 근거

ORD 기록
ord-d30ca6d1de0e4f2e917b81c522cca077
출처 데이터셋
uspto-grants-2008_08
특허 번호
US07417041B2

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