Hydrogen Peroxide → Thieno[3,2-c]isothiazol-3-amine

HRID 332824ノート

反応式

HRID 332824 の反応式
[NH2:1][C:2]1[CH:6]=[CH:5][S:4][C:3]=1[C:7](=[S:9])[NH2:8].OO>CO>[N:1]1[S:9][C:7]([NH2:8])=[C:3]2[S:4][CH:5]=[CH:6][C:2]=12

参加物

4

反応物 2

HCID 784Hydrogen PeroxideHCID 143211023-Amino-2-thiophenecarbothioamide

生成物 1

HCID 818861Thieno[3,2-c]isothiazol-3-amine

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

To a solution of crude 3-aminothiophene-2-carbothioamide in MeOH (5 mL) was added H2O2 (30%, 0.6 mL), after stirring at room temperature for 15 min, it was concentrated to remove most of MeOH, and then diluted with EtOAC, organic layer was washed with brine, concentrated to give crude pdt, purification by column chromatography (DCM/EtOAC=3:1) gave thieno[3,2-c]isothiazol-3-amine (334 mg).

後処理

  1. concentrationit was concentrated
  2. customto remove most of MeOH
  3. additiondiluted with EtOAC, organic layer
  4. washwas washed with brine
  5. concentrationconcentrated
  6. customto give crude
  7. custompdt, purification by column chromatography (DCM/EtOAC=3:1)

出典と根拠

ORDレコード
ord-a1f972cb6cc74047a95768c34fd755ab
出典データセット
uspto-grants-2014_11
特許番号
US08877760B2

反応ノート

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