Ethanol → o-Tolyl thiosemicarbazide

HRID 2071228

反応式

HRID 2071228 の反応式
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]

参加物

5

反応物 3

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

生成物 1

HCID 1490896o-Tolyl thiosemicarbazide

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-99d48bbfe556493a9025b89db86312d9
出典データセット
uspto-grants-1977_09
特許番号
US04046753

関連ノート

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