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

HRID 1455091ノート

反応式

HRID 1455091 の反応式
[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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 3283Diethyl Ether溶媒HCID 6228Dimethylformamide溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-9955c67df08745eb93c40618bc7447cf
出典データセット
uspto-grants-2009_01
特許番号
US07482354B2

反応ノート

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