Potassium Carbonate → HCID 86659718、化合物

HRID 1878552ノート

反応式

HRID 1878552 の反応式
[Cl:1][C:2]1[CH:7]=[C:6](Cl)[N:5]2[N:9]=[C:10]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH:11]=[C:4]2[N:3]=1.Cl.[OH:19][CH:20]1[CH2:23][NH:22][CH2:21]1.C(=O)([O-])[O-].[K+].[K+]>O1CCOCC1>[Cl:1][C:2]1[CH:7]=[C:6]([N:22]2[CH2:23][CH:20]([OH:19])[CH2:21]2)[N:5]2[N:9]=[C:10]([C:12]3[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=3)[CH:11]=[C:4]2[N:3]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 27592903-Hydroxyazetidine hydrochlorideHCID 49761343HCID 49761343、化合物

生成物 1

HCID 86659718HCID 86659718、化合物収率 58%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

There was dissolved, in 1,4-dioxane (2 mL), 5,7-dichloro-2-phenyl-pyrazolo-[1,5-a]pyrimidine (64.5 mg, 0.244 mM), then 3-hydroxy-azetidine hydrochloride (29.4 mg, 0.268 mM) and potassium carbonate (74.2 mg, 0.537 mM) were added to the solution and the mixture was stirred at room temperature for 3 hours. The solvent was removed from this reaction mixture through distillation, the resulting residue was diluted with water and then extracted with methylene chloride. The resulting extracts were combined, dried over anhydrous sodium sulfate, the solvent was distilled off and the resulting solid was washed with diethyl ether to thus give the title compound (42.4 mg, yield: 58%).

後処理

  1. customThe solvent was removed from this reaction mixture through distillation
  2. additionthe resulting residue was diluted with water
  3. extractionextracted with methylene chloride
  4. dry with materialdried over anhydrous sodium sulfate
  5. distillationthe solvent was distilled off
  6. washthe resulting solid was washed with diethyl ether

出典と根拠

ORDレコード
ord-3f5e69dc631d419f9bb7b896f209f585
出典データセット
uspto-grants-2012_11
特許番号
US08314098B2

反応ノート

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