p-Toluenesulfonic acid → HCID 178463002、化合物

HRID 923358ノート

反応式

HRID 923358 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[N:12]=[C:11]([NH2:13])[NH:10][N:9]=1.[CH2:14]([N:16]1[C:24]2[C:19](=[CH:20][C:21]([C:25](=O)[CH2:26][C:27](OCC)=[O:28])=[CH:22][CH:23]=2)[CH:18]=[N:17]1)[CH3:15].CC1C=CC(S(O)(=O)=O)=CC=1>CCCCO>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[C:8]1[N:12]=[C:11]2[NH:13][C:25]([C:21]3[CH:20]=[C:19]4[C:24](=[CH:23][CH:22]=3)[N:16]([CH2:14][CH3:15])[N:17]=[CH:18]4)=[CH:26][C:27](=[O:28])[N:10]2[N:9]=1

参加物

5

反応物 3

HCID 6101p-Toluenesulfonic acidHCID 90109086ethyl 3-(1-ethyl-1H-indazol-5-yl)-3-oxopropanoateHCID 178508279HCID 178508279、化合物

生成物 1

HCID 178463002HCID 178463002、化合物収率 40.4%

試薬・触媒・溶媒 1

HCID 2631-Butanol溶媒

実験手順

To a solution of 3-(2-chlorophenyl)-1H-1,2,4-triazol-5-amine (50 mg, 0.25 mmol) in n-BuOH (0.2 mL) was added ethyl 3-(1-ethyl-1H-indazol-5-yl)-3-oxopropanoate (100 mg, 0.37 mmol) and p-TsOH (10 mg) at room temperature. After refluxing overnight, the solids were collected by filtration and washed with methanol (3×2 mL) to afford 2-(2-chlorophenyl)-5-(1-ethyl-1H-indazol-5-yl)-[1,2,4]triazolo[1,5-α]pyrimidin-7(4H)-one as a yellow solid (39.5 mg, 40%).

後処理

  1. temperatureAfter refluxing overnight
  2. filtrationthe solids were collected by filtration
  3. washwashed with methanol (3×2 mL)

出典と根拠

ORDレコード
ord-35fab2cbde8748ae98f15fff89a1c9f3
出典データセット
uspto-grants-2016_03
特許番号
US09278973B2

反応ノート

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