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

HRID 1811810노트

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HRID 1811810 반응식
[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

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 935Nickel촉매

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온도
70 °C

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-e3c67bd2af2645ab9e9eeb3561e56928
출처 데이터셋
uspto-grants-2013_01
특허 번호
US08362241B2

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