Water → HCID 46836756、化合物

HRID 474222ノート

反応式

HRID 474222 の反応式
Cl[CH2:2][CH:3]([OH:6])[CH2:4][OH:5].C(=O)([O-])[O-].[Cs+].[Cs+].[OH:13][C:14]1[CH:15]=[N:16][C:17]([C:20]2[CH:21]=[C:22]([CH:37]=[CH:38][CH:39]=2)[CH2:23][N:24]2[C:29](=[O:30])[CH:28]=[CH:27][C:26]([C:31]3[CH:32]=[N:33][N:34]([CH3:36])[CH:35]=3)=[N:25]2)=[N:18][CH:19]=1.O>CC(C)=O>[OH:6][CH:3]([CH2:4][OH:5])[CH2:2][O:13][C:14]1[CH:15]=[N:16][C:17]([C:20]2[CH:21]=[C:22]([CH:37]=[CH:38][CH:39]=2)[CH2:23][N:24]2[C:29](=[O:30])[CH:28]=[CH:27][C:26]([C:31]3[CH:32]=[N:33][N:34]([CH3:36])[CH:35]=3)=[N:25]2)=[N:18][CH:19]=1

参加物

6

反応物 4

HCID 962WaterHCID 72903-Chloro-1,2-propanediolHCID 10796Cesium carbonateHCID 59438049HCID 59438049、化合物

生成物 1

HCID 46836756HCID 46836756、化合物

試薬・触媒・溶媒 1

HCID 180Acetone溶媒

反応条件

温度
80 °C

実験手順

75 mg (0.68 mmol) of 3-chloro-1,2-propanediol and 322 mg (0.99 mmol) of caesium carbonate are added to 150 mg (0.41 mmol) of 2-[3-(5-hydroxy-pyrimidin-2-yl)benzyl]-6-(1-methyl-1H-pyrazol-4-yl)-2H-pyridazin-3-one, and the mixture is suspended in acetone. The reaction mixture is stirred at 80° C. for 5 days. Water is added to the reaction mixture, which is then extracted a number of times with ethyl acetate, dried over sodium sulfate and evaporated. The crude product is purified by means of column chromatography on silica gel.

後処理

  1. extractionis then extracted a number of times with ethyl acetate
  2. dry with materialdried over sodium sulfate
  3. customevaporated
  4. customThe crude product is purified by means of column chromatography on silica gel

出典と根拠

ORDレコード
ord-a35ed521ebe442eea318ef75896b3236
出典データセット
uspto-grants-2014_01
特許番号
US08637518B2

反応ノート

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