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

HRID 373914ノート

反応式

HRID 373914 の反応式
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

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 887Methanol溶媒HCID 6342Acetonitrile溶媒

反応条件

温度
50 °C

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-20328215967b47e48bea60c52b3bfce2
出典データセット
uspto-grants-1992_11
特許番号
US05166203

反応ノート

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