Phosgene → 5-(3-Methoxy-4-nitrophenyl)-1,3,4-oxadiazol-2(3H)-one

HRID 722214

反応式

HRID 722214 の反応式
[C:1](Cl)(Cl)=[O:2].[CH3:5][O:6][C:7]1[CH:8]=[C:9]([CH:14]=[CH:15][C:16]=1[N+:17]([O-:19])=[O:18])[C:10]([NH:12][NH2:13])=[O:11]>C1(C)C=CC=CC=1.O1CCOCC1>[CH3:5][O:6][C:7]1[CH:8]=[C:9]([C:10]2[O:11][C:1](=[O:2])[NH:13][N:12]=2)[CH:14]=[CH:15][C:16]=1[N+:17]([O-:19])=[O:18]

参加物

5

反応物 2

HCID 6371PhosgeneHCID 218838753-Methoxy-4-nitrobenzohydrazide

生成物 1

HCID 218839065-(3-Methoxy-4-nitrophenyl)-1,3,4-oxadiazol-2(3H)-one

試薬・触媒・溶媒 2

HCID 1140Toluene溶媒HCID 312751,4-Dioxane溶媒

実験手順

1.2 equivalents of a 20% phosgene solution in toluene were added dropwise to the solution of 850 mg of 3-methoxy-4-nitrobenzoic hydrazide (m.p.: 158.2° C., prepared from methyl 3-methoxy-4-nitrobenzoate and hydrazine hydrate in isopropanol at 80° C.) in 25 ml of dioxane and the mixture was stirred at room temperature for 1 hour. After concentrating, the residue was recrystallized from isopropanol, filtered off with suction and dried under reduced pressure.

後処理

  1. concentrationAfter concentrating
  2. customthe residue was recrystallized from isopropanol
  3. filtrationfiltered off with suction
  4. customdried under reduced pressure

出典と根拠

ORDレコード
ord-2e7b460d44084e60b3df7a9aca359ce1
出典データセット
uspto-grants-2006_11
特許番号
US07138414B2

関連ノート

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