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

HRID 722214

반응식

HRID 722214 반응식
[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]

참가 물질

5

반응물 2

HCID 6371PhosgeneHCID 218838753-Methoxy-4-nitrobenzohydrazide

생성물 1

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

시약·촉매·용매 2

HCID 1140Toluene용매HCID 312751,4-Dioxane용매

실험 절차

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.

후처리

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

출처 및 근거

ORD 기록
ord-2e7b460d44084e60b3df7a9aca359ce1
출처 데이터셋
uspto-grants-2006_11
특허 번호
US07138414B2

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