Potassium thiocyanate → (3-Chloro-2-methylphenyl)thiosemicarbazide
반응식
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]=1참가 물질
4
실험 절차
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.
후처리
- temperaturethe mixture was heated
- temperatureduring reflux for 16 hours
- temperatureThe mixture was then cooled
- customwhereby the product was partially precipitated
- customthe mixture was subsequently evaporated to dryness by means of a rotating evaporator
- customThe product was recrystallized from 200 ml water and 250 ml methanol
- customseparated by filtration
- washwashed thoroughly with water
출처 및 근거
- ORD 기록
- ord-b1c751435ff54ea888fe464c8808333d
- 출처 데이터셋
- uspto-grants-1995_04
- 특허 번호
- US05405857
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