Methylamine → 2-Methoxy-N-methyl-6-[[(methylamino)carbonyl]amino]benzamide

HRID 598070노트

반응식

HRID 598070 반응식
[CH3:1][O:2][C:3]1[C:8]2[C:9](=[O:15])[O:10][C:11]([NH:13][CH3:14])=[N:12][C:7]=2[CH:6]=[CH:5][CH:4]=1.[CH3:16][NH2:17]>CS(C)=O.O>[CH3:1][O:2][C:3]1[CH:4]=[CH:5][CH:6]=[C:7]([NH:12][C:11]([NH:13][CH3:14])=[O:10])[C:8]=1[C:9]([NH:17][CH3:16])=[O:15]

참가 물질

5

반응물 2

HCID 6329MethylamineHCID 672673385-Methoxy-2-(methylamino)-4H-3,1-benzoxazin-4-one

생성물 1

HCID 672680242-Methoxy-N-methyl-6-[[(methylamino)carbonyl]amino]benzamide수율 81.2%

시약·촉매·용매 2

HCID 679Dimethyl Sulfoxide용매HCID 962Water용매

실험 절차

A mixture of 5-Methoxy-2-(methylamino)-4H-3,1-benzoxazin-4-one (1.05 g, 5.09 mmol) and methylamine (2.0 M solution in tetrahydrofuran; 12.7 ml, 25.5 mmol) in dimethylsulfoxide (2 ml) was heated in sealed tube for 15 h. After cooling, the mixture was diluted with water and extracted with ethyl acetate. The extract was washed with brine, dried over magnesium sulfate and concentrated under vacuum to afford 0.980 g (81%) of the title compound.

후처리

  1. temperaturewas heated in sealed tube for 15 h
  2. temperatureAfter cooling
  3. extractionextracted with ethyl acetate
  4. washThe extract was washed with brine
  5. dry with materialdried over magnesium sulfate
  6. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-1c3147244f144c97b697d37526ea4b92
출처 데이터셋
uspto-grants-2011_03
특허 번호
US07897607B2

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