Potassium thiocyanate → (3-Chloro-2-methylphenyl)thiosemicarbazide

HRID 1654068ノート

反応式

HRID 1654068 の反応式
Cl.[Cl:2][C:3]1[C:4]([CH3:11])=[C:5]([NH:9][NH2:10])[CH:6]=[CH:7][CH:8]=1.[S-:12][C:13]#[N:14].[K+]>C(O)C>[Cl:2][C:3]1[C:4]([CH3:11])=[C:5]([NH:9][NH:10][C:13]([NH2:14])=[S:12])[CH:6]=[CH:7][CH:8]=1

参加物

4

反応物 2

HCID 516872Potassium thiocyanateHCID 12732296(3-Chloro-2-methylphenyl)hydrazine hydrochloride

生成物 1

HCID 20079518(3-Chloro-2-methylphenyl)thiosemicarbazide

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

19.3 g (0.1 mole) of 3-chloro-2-methylphenylhydrazinehydrochloride were dissolved in 200 ml of absolute ethanol. 11.64 g (0.12 mole) of potassium thiocyanate were added to the solution, and the mixture was heated during reflux for 16 hours. The mixture was then cooled, whereby the product was partially precipitated, and the mixture was subsequently evaporated to dryness by means of a rotating evaporator. The product was recrystallized from 200 ml water and 250 ml methanol, separated by filtration and washed thoroughly with water.

後処理

  1. temperaturethe mixture was heated
  2. temperatureduring reflux for 16 hours
  3. temperatureThe mixture was then cooled
  4. customwhereby the product was partially precipitated
  5. customthe mixture was subsequently evaporated to dryness by means of a rotating evaporator
  6. customThe product was recrystallized from 200 ml water and 250 ml methanol
  7. customseparated by filtration
  8. washwashed thoroughly with water

出典と根拠

ORDレコード
ord-b1c751435ff54ea888fe464c8808333d
出典データセット
uspto-grants-1995_04
特許番号
US05405857

反応ノート

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