Ethanol → 2-(2-Fluoro-5-((4-(methylsulfonyl)piperazin-1-YL)methyl)pyridin-3-YL)-4-methyl-1,3,5-triazine

HRID 1621398ノート

反応式

HRID 1621398 の反応式
[F:1][C:2]1[C:7]([C:8]2[N:13]=[C:12]([CH3:14])[N:11]=[C:10](SC)[N:9]=2)=[CH:6][C:5]([CH2:17][N:18]2[CH2:23][CH2:22][N:21]([S:24]([CH3:27])(=[O:26])=[O:25])[CH2:20][CH2:19]2)=[CH:4][N:3]=1.CCO>[Ni]>[F:1][C:2]1[C:7]([C:8]2[N:13]=[C:12]([CH3:14])[N:11]=[CH:10][N:9]=2)=[CH:6][C:5]([CH2:17][N:18]2[CH2:19][CH2:20][N:21]([S:24]([CH3:27])(=[O:26])=[O:25])[CH2:22][CH2:23]2)=[CH:4][N:3]=1

参加物

4

反応物 2

HCID 702EthanolHCID 595481882-(2-Fluoro-5-((4-(methylsulfonyl)piperazin-1-yl)methyl)pyridin-3-yl)-4-methyl-6-(methylthio)-1,3,5-triazine

生成物 1

HCID 666005952-(2-Fluoro-5-((4-(methylsulfonyl)piperazin-1-YL)methyl)pyridin-3-YL)-4-methyl-1,3,5-triazine

試薬・触媒・溶媒 1

HCID 935Nickel触媒

反応条件

温度
70 °C

実験手順

Raney nickel (76 mg, 1.297 mmol) water suspension was added to a mixture of 2-(2-fluoro-5-((4-(methylsulfonyl)piperazin-1-yl)methyl)pyridin-3-yl)-4-methyl-6-(methylthio)-1,3,5-triazine (107 mg, 0.259 mmol) in EtOH (5.00 mL, 86 mmol) and the mixture was heated under nitrogen at 70° C. for 1.5 h. The resulting mixture was passed through a short plug of Celite® (diatomaceous earth). The filter cake was washed with MeOH (3×10 mL). The combined organic phases were concentrated to give the crude product, which was used directly in the next step without purification.

後処理

  1. washThe filter cake was washed with MeOH (3×10 mL)
  2. concentrationThe combined organic phases were concentrated

出典と根拠

ORDレコード
ord-bb79c404cb074dcc8614ab2b7e3d5694
出典データセット
uspto-grants-2014_07
特許番号
US08772480B2

反応ノート

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