Water → 1-methyl-8-(methylsulfonyl)-4,5-dihydro-1H-pyrazolo[4,3-h]quinazoline-3-carboxamide

HRID 44581노트

반응식

HRID 44581 반응식
[CH3:1][N:2]1[C:14]2[C:13]3[N:12]=[C:11](SC)[N:10]=[CH:9][C:8]=3[CH2:7][CH2:6][C:5]=2[C:4]([C:17]([NH2:19])=[O:18])=[N:3]1.O[O:21][S:22]([O-:24])=O.[K+].O.[C:27](OCC)(=O)C>CN(C)C=O.C(OCC)C>[CH3:1][N:2]1[C:14]2[C:13]3[N:12]=[C:11]([S:22]([CH3:27])(=[O:24])=[O:21])[N:10]=[CH:9][C:8]=3[CH2:7][CH2:6][C:5]=2[C:4]([C:17]([NH2:19])=[O:18])=[N:3]1

참가 물질

7

반응물 4

HCID 962WaterHCID 8857Ethyl AcetateHCID 23707502Potassium hydroxy sulfiteHCID 451416071-methyl-8-(methylthio)-4,5-dihydro-1H-pyrazolo[4,3-h]quinazoline-3-carboxamide

생성물 1

HCID 116524591-methyl-8-(methylsulfonyl)-4,5-dihydro-1H-pyrazolo[4,3-h]quinazoline-3-carboxamide수율 80%

시약·촉매·용매 2

HCID 3283Diethyl Ether용매HCID 6228Dimethylformamide용매

실험 절차

6.00 g (0.022 mol) of 1-methyl-8-(methylthio)-4,5-dihydro-1H-pyrazolo[4,3-h]quinazoline-3-carboxamide were dissolved in 1000 mL of dimethylformamide and 40.18 g of oxone were added. The mixture was stirred 16 hours at room temperature. Water and ethyl acetate were then added and the layers separated. The organic layer was finally dried over Na2SO4 and evaporated. The residue was triturated with diethyl ether and 5.40 g (80% yield) of the title compound were collected by filtration.

후처리

  1. customthe layers separated
  2. dry with materialThe organic layer was finally dried over Na2SO4
  3. customevaporated

출처 및 근거

ORD 기록
ord-3a0ea2666ae942e2a9a4d318ba0a926a
출처 데이터셋
uspto-grants-2013_09
특허 번호
US08541429B2

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