Lawesson's reagent → HCID 86649596、化合物

HRID 1530054ノート

反応式

HRID 1530054 の反応式
[CH2:1]([N:3]1[CH:7]=[C:6]([C:8]([NH2:10])=O)[C:5]([CH3:11])=[N:4]1)[CH3:2].COC1C=CC(P2(SP(C3C=CC(OC)=CC=3)(=S)S2)=[S:21])=CC=1>C1(C)C=CC=CC=1>[CH2:1]([N:3]1[CH:7]=[C:6]([C:8](=[S:21])[NH2:10])[C:5]([CH3:11])=[N:4]1)[CH3:2]

参加物

4

反応物 2

HCID 87949Lawesson's reagentHCID 49949164HCID 49949164、化合物

生成物 1

HCID 86649596HCID 86649596、化合物収率 24%

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

To a suspension of 1-ethyl-3-methyl-1H-pyrazole-4-carboxamide (1.7 g, 11 mmol) produced in the above in toluene (80 mL) was added Lawesson's reagent (7.0 g, 17 mmol), and the mixture was heated under reflux for 1.5 hr. The reaction solution was cooled to room temperature and purified by basic silica gel column chromatography (ethyl acetate/hexane=0/100→20/80) to give the title compound (445 mg, 24%) as a yellow oil.

後処理

  1. temperaturethe mixture was heated
  2. temperatureunder reflux for 1.5 hr
  3. custompurified by basic silica gel column chromatography (ethyl acetate/hexane=0/100→20/80)

出典と根拠

ORDレコード
ord-c015e4199df84b3fa1780e2e724f026b
出典データセット
uspto-grants-2015_07
特許番号
US09090601B2

反応ノート

読み込み中…