Water → 2-[3-(5-bromopyrimidin-2-yl)benzyl]-6-phenoxy-2H-pyridazin-3-one

HRID 532418ノート

反応式

HRID 532418 の反応式
[Br:1][C:2]1[CH:3]=[N:4][C:5]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([CH2:14]Cl)[CH:9]=2)=[N:6][CH:7]=1.C(=O)([O-])[O-].[Cs+].[Cs+].[O:22]([C:29]1[CH:30]=[CH:31][C:32](=[O:35])[NH:33][N:34]=1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1.O>CN(C=O)C>[Br:1][C:2]1[CH:3]=[N:4][C:5]([C:8]2[CH:9]=[C:10]([CH:11]=[CH:12][CH:13]=2)[CH2:14][N:33]2[C:32](=[O:35])[CH:31]=[CH:30][C:29]([O:22][C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)=[N:34]2)=[N:6][CH:7]=1

参加物

6

反応物 4

HCID 962WaterHCID 10796Cesium carbonateHCID 468893056-phenoxypyridazin-3(2H)-oneHCID 594380475-Bromo-2-(3-(chloromethyl)phenyl)pyrimidine

生成物 1

HCID 584970712-[3-(5-bromopyrimidin-2-yl)benzyl]-6-phenoxy-2H-pyridazin-3-one

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

3.3 2.59 g (9.14 mmol) of 5-bromo-2-(3-chloromethylphenyl)pyrimidine and 2.84 g (8.70 mmol) of caesium carbonate are added to a suspension of 1.64 g (8.70 mmol) of 6-phenoxy-2H-pyridazin-3-one in 17.5 ml of DMF, and the mixture is stirred at room temperature for 18 hours. Water is added to the reaction mixture. The precipitate formed is filtered off with suction, washed with water and dried in vacuo, giving 2-[3-(5-bromopyrimidin-2-yl)benzyl]-6-phenoxy-2H-pyridazin-3-one as colourless crystals; ESI 435, 437.

後処理

  1. customThe precipitate formed
  2. filtrationis filtered off with suction
  3. washwashed with water
  4. customdried in vacuo

出典と根拠

ORDレコード
ord-f15b5bad386c4d36901c05cc26fe441d
出典データセット
uspto-grants-2014_10
特許番号
US08853211B2

反応ノート

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