Ethanol → o-Tolyl thiosemicarbazide

HRID 2071228

반응식

HRID 2071228 반응식
Cl.[C:2]1([CH3:10])[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][NH2:9].[S-:11][C:12]#[N:13].[NH4+].C(O)C>O>[C:2]1([CH3:10])[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[NH:8][NH:9][C:12]([NH2:13])=[S:11]

참가 물질

5

반응물 3

HCID 702EthanolHCID 15666Ammonium thiocyanateHCID 71554o-Tolylhydrazinium(1+) chloride

생성물 1

HCID 1490896o-Tolyl thiosemicarbazide

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 15.9 g. (0.1 moles) of o-tolylhydrazine hydrochloride, 15.2 g. (0.2 moles) of ammonium thiocyanate, 300 ml. of ethanol and 30 ml. of water are heated at reflux temperature for 24 hours, the solvent is removed by distillation at atmospheric pressure, and sufficient water added to cause precipitation. The aqueous suspension is filtered and the solid residue recrystallized from aqueous ethanol affording 15 g. (85%) of 1-(o-tolyl)-3-thiosemicarbazide, m.p. 158°-160° C.

후처리

  1. additionA mixture of 15.9 g
  2. temperatureat reflux temperature for 24 hours
  3. customthe solvent is removed by distillation at atmospheric pressure, and sufficient water
  4. additionadded
  5. customprecipitation
  6. filtrationThe aqueous suspension is filtered
  7. customthe solid residue recrystallized from aqueous ethanol affording 15 g

출처 및 근거

ORD 기록
ord-99d48bbfe556493a9025b89db86312d9
출처 데이터셋
uspto-grants-1977_09
특허 번호
US04046753

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