Methanol → 1-Methyl-3,5-diphenylpyrazole

HRID 357529

反応式

HRID 357529 の反応式
[CH3:1]O.[C:3]1([C:9]2[CH:13]=[C:12]([C:14]3[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=3)[NH:11][N:10]=2)[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=1>OS(O)(=O)=O>[CH3:1][N:10]1[C:9]([C:3]2[CH:8]=[CH:7][CH:6]=[CH:5][CH:4]=2)=[CH:13][C:12]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)=[N:11]1

参加物

4

反応物 2

HCID 887MethanolHCID 708401H-Pyrazole, 3,5-diphenyl-

生成物 1

HCID 1405171-Methyl-3,5-diphenylpyrazole収率 95.7%

試薬・触媒・溶媒 1

HCID 1118Sulfuric Acid触媒

実験手順

308.5 g (9.64 mol) of methanol were vaporized dropwise at 155° C. in an electrically heated column with a diameter of 4 cm and equipped with a sintered disk at the lower end and fitted onto a 250 ml two-neck flask over the course of 6 hours and passed through a melt, at 200° C., of 10 g (0.0455 mol) of 3,5-diphenylpyrazole and 0.046 g (0.000455 mol) of concentrated H2SO4. The gaseous discharge from the reaction was condensed and concentrated under reduced pressure. 10.2 g (92.5%) of 1-methyl-3,5-diphenylpyrazole were obtained, boiling point 190° C./3 mbar, with a content of 96.6% (GC).

後処理

  1. customwere vaporized dropwise at 155° C. in an electrically heated column with a diameter of 4 cm
  2. customequipped with a sintered disk at the lower end
  3. customfitted onto a 250 ml two-neck flask over the course of 6 hours
  4. customcondensed
  5. concentrationconcentrated under reduced pressure

出典と根拠

ORDレコード
ord-124fcfbe4b81403490c59dcf5beb8fe0
出典データセット
uspto-grants-1998_11
特許番号
US05840913

関連ノート

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