Hydrochloric Acid → HCID 11660878、化合物

HRID 2192195ノート

反応式

HRID 2192195 の反応式
[NH2:1][C:2]1[CH:19]=[C:18]([F:20])[C:5]([O:6][C:7]2[CH:12]=[CH:11][N:10]=[C:9]3[NH:13][CH:14]=[C:15]([C:16]#[N:17])[C:8]=23)=[C:4]([F:21])[CH:3]=1.Cl[C:23]1[CH:28]=[CH:27][N:26]=[C:25]([NH2:29])[N:24]=1.Cl.[OH-].[Na+]>O.C(O)C>[NH2:29][C:25]1[N:26]=[C:27]([NH:1][C:2]2[CH:19]=[C:18]([F:20])[C:5]([O:6][C:7]3[CH:12]=[CH:11][N:10]=[C:9]4[NH:13][CH:14]=[C:15]([C:16]#[N:17])[C:8]=34)=[C:4]([F:21])[CH:3]=2)[CH:28]=[CH:23][N:24]=1

参加物

7

反応物 4

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 2233322-Amino-4-chloropyrimidineHCID 59740983HCID 59740983、化合物

生成物 1

HCID 11660878HCID 11660878、化合物

試薬・触媒・溶媒 2

HCID 702Ethanol溶媒HCID 962Water溶媒2 回

実験手順

250 mg (0.65 mmol) of 4-(4-amino-2,6-difluorophenoxy)-1H-pyrrolo[2,3-b]pyridine-3-carbonitrile and 92 mg (0.71 mmol) of 4-chloropyrimidine-2-amine are suspended in 10 ml of water and 5 ml of ethanol. 0.32 ml (1.29 mmol) of 4N hydrochloric acid is added, and the mixture is heated at reflux for 2 h. The mixture is made alkaline using concentrated aqueous sodium hydroxide solution, diluted with water and extracted with ethyl acetate. The organic phase is separated off and concentrated. The crude product is purified by preparative HPLC. This gives the title compound as crystals.

後処理

  1. temperaturethe mixture is heated
  2. temperatureat reflux for 2 h
  3. extractionextracted with ethyl acetate
  4. customThe organic phase is separated off
  5. concentrationconcentrated
  6. customThe crude product is purified by preparative HPLC

出典と根拠

ORDレコード
ord-96da8a147eb0402082ce02d18d729319
出典データセット
uspto-grants-2012_12
特許番号
US08329716B2

反応ノート

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