Phenoxyethanol → 3-(2-phenoxyethoxy)-1H-pyrazol-5-amine

HRID 1878550

반응식

HRID 1878550 반응식
[NH2:1][C:2]1[NH:6][N:5]=[C:4]([OH:7])[CH:3]=1.O.C1(C)C=CC(S(O)(=O)=O)=CC=1.[O:20]([CH2:27][CH2:28]O)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1>C(#N)C>[O:20]([CH2:27][CH2:28][O:7][C:4]1[CH:3]=[C:2]([NH2:1])[NH:6][N:5]=1)[C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][CH:22]=1

참가 물질

5

반응물 3

HCID 31236PhenoxyethanolHCID 521998p-Toluenesulfonic acid monohydrateHCID 178507967HCID 178507967, 화합물

생성물 1

HCID 189815973-(2-phenoxyethoxy)-1H-pyrazol-5-amine수율 33%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
130 °C

실험 절차

There was suspended, in 2-phenoxy ethanol (25 g, 180 mM), 5-amino-1H-pyrazol-3-ol (4.00 g, 41.4 mM), then p-toluenesulfonic acid monohydrate (15.4 g, 80.8 mM) was added to the suspension and the mixture was stirred at 130° C. for 5 hours under reduced pressure. This reaction liquid was diluted with acetonitrile, the solid precipitated out of the liquid was filtered off and washed with acetonitrile. The resulting solid was suspended in a 6% aqueous sodium bicarbonate solution (250 mL), the suspension was stirred at room temperature and the solid was then filtered off. The resulting solid was dissolved in ethyl acetate, dried over anhydrous sodium sulfate and then the solvent was distilled off to thus give the title compound (2.90 g, yield: 33%).

후처리

  1. customThis reaction liquid
  2. customthe solid precipitated out of the liquid
  3. filtrationwas filtered off
  4. washwashed with acetonitrile
  5. stirringthe suspension was stirred at room temperature
  6. filtrationthe solid was then filtered off
  7. dissolutionThe resulting solid was dissolved in ethyl acetate
  8. dry with materialdried over anhydrous sodium sulfate
  9. distillationthe solvent was distilled off

출처 및 근거

ORD 기록
ord-19d64cded8924a4db4d3cb715631a67a
출처 데이터셋
uspto-grants-2012_11
특허 번호
US08314098B2

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