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Water → 4-iodo-1H-indazol-3-amine

HRID 497602
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HRID 497602 반응식
O.[NH2:2][NH2:3].F[C:5]1[CH:12]=[CH:11][CH:10]=[C:9]([I:13])[C:6]=1[C:7]#[N:8].O>C(O)C>[I:13][C:9]1[CH:10]=[CH:11][CH:12]=[C:5]2[C:6]=1[C:7]([NH2:8])=[N:2][NH:3]2
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962WaterHCID 24654Hydrazine hydrate (1:1)HCID 5227222-Fluoro-6-iodobenzonitrile

생성물 1

HCID 40577874-iodo-1H-indazol-3-amine

시약·촉매·용매 1

HCID 702Ethanol용매

반응 조건

온도
78 °C

실험 절차

1.2 cm3 of hydrazine monohydrate are added to 2 g of 2-fluoro-6-iodobenzonitrile in 25 cm3 of ethanol. The reaction medium is then refluxed at about 78° C. for 12 hours. The medium is allowed to return to about 20° C. and 20 cm 3 of distilled water are then added in order to precipitate the product. The insoluble material is filtered on a sinter funnel, rinsed with 20 cm3 of distilled water and then taken up in 20 cm3 of dichloromethane. The organic phase is then dried over magnesium sulphate and evaporated under reduced pressure (2 kPa; 45° C.). After drying (90 Pa; 50° C.), 1.65 g of 4-iodo-1H-indazole-3-amine are obtained in the form of a yellow solid melting at 157° C.

이 페이지에서참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

후처리

  1. customto return to about 20° C.
  2. customto precipitate the product
  3. filtrationThe insoluble material is filtered on a sinter funnel
  4. washrinsed with 20 cm3 of distilled water
  5. dry with materialThe organic phase is then dried over magnesium sulphate
  6. customevaporated under reduced pressure (2 kPa; 45° C.)
  7. dry with materialAfter drying (90 Pa; 50° C.), 1.65 g of 4-iodo-1H-indazole-3-amine

출처 및 근거

ORD 기록
ord-2ae53273fb014e0881c0daf7302f8d3a
출처 데이터셋
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06949579B2

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