Piperazine → 2-(3-Fluoro-phenyl)-5-piperazin-1-yl-[1,2,4]triazolo[1,5-a][1,3,5]triazin-7-ylamine

HRID 1181296노트

반응식

HRID 1181296 반응식
[F:1][C:2]1[CH:3]=[C:4]([C:8]2[N:21]=[C:11]3[N:12]=[C:13](S(C)(=O)=O)[N:14]=[C:15]([NH2:16])[N:10]3[N:9]=2)[CH:5]=[CH:6][CH:7]=1.[NH:22]1[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]1>CC#N>[F:1][C:2]1[CH:3]=[C:4]([C:8]2[N:21]=[C:11]3[N:12]=[C:13]([N:22]4[CH2:27][CH2:26][NH:25][CH2:24][CH2:23]4)[N:14]=[C:15]([NH2:16])[N:10]3[N:9]=2)[CH:5]=[CH:6][CH:7]=1

참가 물질

4

반응물 2

HCID 4837PiperazineHCID 694324922-(3-Fluoro-phenyl)-5-methanesulfonyl-[1,2,4]triazolo[1,5-a][1,3,5]triazin-7-ylamine

생성물 1

HCID 694310402-(3-Fluoro-phenyl)-5-piperazin-1-yl-[1,2,4]triazolo[1,5-a][1,3,5]triazin-7-ylamine

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

18 mmol of 2-(3-fluoro-phenyl)-5-methanesulfonyl-[1,2,4]triazolo[1,5-a][1,3,5]triazin-7-ylamine (prepared as described Caulkett et al., J. Chem. Soc. Perkin Trans I. 801-808 (1995)) was suspended in 50 mL of CH3CN along with 5 eq. of piperazine. The reaction mixture was stirred under reflux for 2 hours. It was then cooled to room temperature and concentrated under reduced pressure. The residue was taken up in CH2Cl2 and washed with H2O, brine, dried with Na2SO4, and concentrated under reduced pressure. The resulting crude product was purified by chromatography (95% CH2Cl2, 4% MeOH, 1% Et3N) to afford 2-(3-fluoro-phenyl)-5-piperazin-1-yl-[1,2,4]triazolo[1,5-a][1,3,5]triazin-7-ylamine.

후처리

  1. temperatureunder reflux for 2 hours
  2. concentrationconcentrated under reduced pressure
  3. washwashed with H2O, brine
  4. dry with materialdried with Na2SO4
  5. concentrationconcentrated under reduced pressure
  6. customThe resulting crude product was purified by chromatography (95% CH2Cl2, 4% MeOH, 1% Et3N)

출처 및 근거

ORD 기록
ord-56979c4955aa42538d2f1f2239778906
출처 데이터셋
uspto-grants-2007_10
특허 번호
US07285550B2

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