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Potassium Carbonate → 6-(2,6-dichlorobenzoylamino)-2,3-dihydro-1-methyl-2-(pyridin-4-ylmethyl)-1H-pyrazolo[4,3-c]quinolin-3-one

HRID 613481
ノート
印刷プレビュー

反応式

HRID 613481 の反応式
Cl.[Cl:2][C:3]1[CH:26]=[CH:25][CH:24]=[C:23]([Cl:27])[C:4]=1[C:5]([NH:7][C:8]1[C:17]2[N:16]=[CH:15][C:14]3[C:18](=[O:22])[NH:19][N:20]([CH3:21])[C:13]=3[C:12]=2[CH:11]=[CH:10][CH:9]=1)=[O:6].Cl.Cl[CH2:30][C:31]1[CH:36]=[CH:35][N:34]=[CH:33][CH:32]=1.C(=O)([O-])[O-].[K+].[K+]>CN(C)C=O>[Cl:27][C:23]1[CH:24]=[CH:25][CH:26]=[C:3]([Cl:2])[C:4]=1[C:5]([NH:7][C:8]1[C:17]2[N:16]=[CH:15][C:14]3[C:18](=[O:22])[N:19]([CH2:30][C:31]4[CH:36]=[CH:35][N:34]=[CH:33][CH:32]=4)[N:20]([CH3:21])[C:13]=3[C:12]=2[CH:11]=[CH:10][CH:9]=1)=[O:6]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 745704-(Chloromethyl)pyridinium chlorideHCID 195929636-(2,6-dichlorobenzoylamino)-2,3-dihydro-1-methyl-1H-pyrazolo[4,3-c]quinolin-3-one hydrochloride

生成物 1

HCID 195924656-(2,6-dichlorobenzoylamino)-2,3-dihydro-1-methyl-2-(pyridin-4-ylmethyl)-1H-pyrazolo[4,3-c]quinolin-3-one

試薬・触媒・溶媒 1

HCID 6228
Dimethylformamide
溶媒

実験手順

A mixture of 6-(2,6-dichlorobenzoylamino)-2,3-dihydro-1-methyl-1H-pyrazolo[4,3-c]quinolin-3-one hydrochloride (85 mg), 4-chloromethylpyridine hydrochloride (40 mg) and potassium carbonate (111 mg) in dimethylformamide (1 ml) was stirred for 3 hours at ambient temperature. The mixture was partitioned between ethyl acetate and water. The organic layer was washed with brine, dried over magnesium sulfate and evaporated in vacuo. The residue was purified by column chromatography on silica gel to give 6-(2,6-dichlorobenzoylamino)-2,3-dihydro-1-methyl-2-(pyridin-4-ylmethyl)-1H-pyrazolo[4,3-c]quinolin-3-one.

後処理

  1. customThe mixture was partitioned between ethyl acetate and water
  2. washThe organic layer was washed with brine
  3. dry with materialdried over magnesium sulfate
  4. customevaporated in vacuo
  5. customThe residue was purified by column chromatography on silica gel

出典と根拠

ORDレコード
ord-01452a8e5e7d4b87b305005f99133782
出典データセット
uspto-grants-1999_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06008230

反応ノート

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