NBD-Cl → 7-Chloro-2,1,3-benzoxadiazol-4-amine

HRID 966901

반응식

HRID 966901 반응식
[Cl:1][C:2]1[C:7]2=[N:8][O:9][N:10]=[C:6]2[C:5]([N+:11]([O-])=O)=[CH:4][CH:3]=1>CC(O)=O.CCOC(C)=O.O.[Fe]>[NH2:11][C:5]1[C:6]2[C:7](=[N:8][O:9][N:10]=2)[C:2]([Cl:1])=[CH:3][CH:4]=1

참가 물질

6

반응물 1

HCID 25043NBD-Cl

생성물 1

HCID 218751677-Chloro-2,1,3-benzoxadiazol-4-amine수율 94%

시약·촉매·용매 4

HCID 23925Iron촉매HCID 176Acetic Acid용매HCID 962Water용매HCID 8857Ethyl Acetate용매

반응 조건

온도
80 °C

실험 절차

A solution of 1.0 g (5.02 mmol) of 4-chloro-7-nitrobenzofurazan in 20 mL AcOH, 10 mL EtOAc and 2 mL H2O was heated at 50° C. and treated with iron powder (1.4 g, 251 mmol). The mixture was heated at 80° C. for 30 min and then allowed to cool to rt. The mixture was filtered through Celite eluting with EtOAc. The filtrate was washed with sat. aq. NaHCO3, dried over MgSO4, and concentrated under reduced pressure to give compound 258A (0.80 g, 94%) as a red solid.

후처리

  1. temperatureto cool to rt
  2. filtrationThe mixture was filtered through Celite
  3. washeluting with EtOAc
  4. washThe filtrate was washed with sat. aq. NaHCO3
  5. dry with materialdried over MgSO4
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-26a2fc2eb88d4fbca4c90a503bb6f641
출처 데이터셋
uspto-grants-2005_10
특허 번호
US06953679B2

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