Water → HCID 67260840、化合物

HRID 2359043ノート

反応式

HRID 2359043 の反応式
C([NH:8][C:9]1[N:14]=[C:13]([C:15]2[C:16]([C:23]3[S:24][C:25]([Cl:28])=[CH:26][CH:27]=3)=[N:17][N:18]([CH:20]([CH3:22])[CH3:21])[CH:19]=2)[CH:12]=[CH:11][N:10]=1)C1C=CC=CC=1.O.[OH-].[Na+]>S(=O)(=O)(O)O>[Cl:28][C:25]1[S:24][C:23]([C:16]2[C:15]([C:13]3[CH:12]=[CH:11][N:10]=[C:9]([NH2:8])[N:14]=3)=[CH:19][N:18]([CH:20]([CH3:22])[CH3:21])[N:17]=2)=[CH:27][CH:26]=1

参加物

5

反応物 3

HCID 962WaterHCID 14798Sodium HydroxideHCID 67261084HCID 67261084、化合物

生成物 1

HCID 67260840HCID 67260840、化合物収率 55.5%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid溶媒

実験手順

A mixture of N-benzyl-4-[3-(5-chloro-2-thienyl)-1-isopropyl-1H-pyrazol-4-yl]pyrimidin-2-amine (1 eq, 3.1 mmol) in 11 mL sulfuric acid was stirred at room temperature overnight. Ice was added followed by water and a solution of NaOH 30% until pH=9. The aqueous layer was extracted with dichloromethane and the combined organic extracts were dried over MgSO4 filtered and concentrated to afford 0.55 g of 4-[3-(5-chloro-2-thienyl)-1-isopropyl-1H-pyrazol-4-yl]pyrimidin-2-amine (50% yield).

後処理

  1. additionIce was added
  2. extractionThe aqueous layer was extracted with dichloromethane
  3. dry with materialthe combined organic extracts were dried over MgSO4
  4. filtrationfiltered
  5. concentrationconcentrated

出典と根拠

ORDレコード
ord-26f02fa6538a4d438475e6319514e3d6
出典データセット
uspto-grants-2014_04
特許番号
US08685974B2

反応ノート

読み込み中…