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Dichloromethane → 6-fluoro-1H-indazol-5-amine

HRID 227717
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HRID 227717 반응식
[F:1][C:2]1[CH:10]=[C:9]2[C:5]([CH:6]=[N:7][NH:8]2)=[CH:4][C:3]=1[N+:11]([O-])=O.C(Cl)Cl.[H][H]>[Pd].CO>[F:1][C:2]1[CH:10]=[C:9]2[C:5]([CH:6]=[N:7][NH:8]2)=[CH:4][C:3]=1[NH2:11]
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참가 물질

6

반응물 3

HCID 6344DichloromethaneHCID 459336676-Fluoro-5-nitro-1H-indazoleHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 450905046-fluoro-1H-indazol-5-amine수율 75%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

To the product of Step (c) (530 mg, 2.93 mmol, 1 equiv) and 10% Pd/C (200 mg) was added CH2Cl2 (10 mL) and MeOH (40 mL). The atmosphere was replaced with hydrogen gas and the solution was stirred at room temperature and atmospheric pressure for 2 hours. The reaction mixture was filtered through a plug of celite and rinsed with MeOH and CH2Cl2. The residue was purified by flash chromatography (linear gradient, 40→70% EtOAc/hexanes) affording 330 mg (75%) of the title compound as a pale purple solid. MS (ES+) m/e 152 [M+H].

후처리

  1. filtrationThe reaction mixture was filtered through a plug of celite
  2. washrinsed with MeOH and CH2Cl2
  3. customThe residue was purified by flash chromatography (linear gradient, 40→70% EtOAc/hexanes)

출처 및 근거

ORD 기록
ord-615325a38229463e82c38a74f1860b59
출처 데이터셋
uspto-grants-2009_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07560467B2

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