Methylamine → 5-methyl-6,7-difluoro-1H,4H-thiazolo[3,4-a]quinoxaline-1-thione

HRID 373914노트

반응식

HRID 373914 반응식
Cl[CH2:2][C:3]1[N:4]([C:9]2[CH:14]=[CH:13][C:12]([F:15])=[C:11]([F:16])[C:10]=2F)[C:5](=[S:8])[S:6][CH:7]=1.[CH3:18][NH2:19]>C(#N)C.CO>[CH3:18][N:19]1[C:10]2[C:9](=[CH:14][CH:13]=[C:12]([F:15])[C:11]=2[F:16])[N:4]2[C:5](=[S:8])[S:6][CH:7]=[C:3]2[CH2:2]1

참가 물질

5

반응물 2

HCID 6329MethylamineHCID 41903592(3H)-Thiazolethione, 4-(chloromethyl)-3-(2,3,4-trifluorophenyl)-

생성물 1

HCID 104683535-methyl-6,7-difluoro-1H,4H-thiazolo[3,4-a]quinoxaline-1-thione

시약·촉매·용매 2

HCID 887Methanol용매HCID 6342Acetonitrile용매

반응 조건

온도
50 °C

실험 절차

4-Chloromethyl-3-(2,3,4-trifluorophenyl)-2(3H)-thiazolethione (2.5 g) is dissolved in acetonitrile (25 ml) and thereto is added 40% solution of methylamine in methanol (3.3 g), and the mixture is stirred at 50° C. for 16 hours. The reaction mixture is evaporated to dryness under reduced pressure, and water is added to the residue and the mixture is extracted with chloroform. The extract is washed with saline solution, dried over anhydrous sodium sulfate and distilled under reduced pressure to remove the solvent. The residue is recrystallized from cyclohexane-ethyl acetate to give the title compound (2.0 g) as yellow crystals.

후처리

  1. customThe reaction mixture is evaporated to dryness under reduced pressure, and water
  2. additionis added to the residue
  3. extractionthe mixture is extracted with chloroform
  4. washThe extract is washed with saline solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. distillationdistilled under reduced pressure
  7. customto remove the solvent
  8. customThe residue is recrystallized from cyclohexane-ethyl acetate

출처 및 근거

ORD 기록
ord-20328215967b47e48bea60c52b3bfce2
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05166203

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