Cyclohexyl isothiocyanate → Hydrazinecarbothioamide, 2-(1-(2-pyridinyl)ethylidene)-

HRID 1198396ノート

反応式

HRID 1198396 の反応式
[C:1](=[N:9][NH2:10])([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1)[CH3:2].C1([N:17]=[C:18]=[S:19])CCCCC1>CO>[C:1](=[N:9][NH:10][C:18]([NH2:17])=[S:19])([C:3]1[CH:8]=[CH:7][CH:6]=[CH:5][N:4]=1)[CH3:2]

参加物

4

反応物 2

HCID 14289Cyclohexyl isothiocyanateHCID 474761HCID 474761、化合物

生成物 1

HCID 2732427Hydrazinecarbothioamide, 2-(1-(2-pyridinyl)ethylidene)-収率 46%

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

A solution of 6.76 g (0.05 mol) of 2-acetylpyridine hydrazone in 10 ml of MeOH was treated with 7.2 g (0.05 mol) of cyclohexyl isothiocyanate and the solution was heated at reflux for 3 hours. The solution was chilled, and the crystals which formed were collected. Recrystallization of the product from 150 ml of MeOH afforded 6.40 9 (46%) of white needles of 2-acetylpyridine 4-cyclohexyl-3-thiosemicarbazone, mp 155° C.

後処理

  1. temperaturethe solution was heated
  2. temperatureat reflux for 3 hours
  3. temperatureThe solution was chilled
  4. customthe crystals which formed
  5. customwere collected
  6. customRecrystallization of the product from 150 ml of MeOH

出典と根拠

ORDレコード
ord-ba56af65238d4592aef5b948ea14edf2
出典データセット
uspto-grants-1994_01
特許番号
US05281597

反応ノート

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