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6-Nitro-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-indazole → HCID 67293196, 화합물

HRID 1038860
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HRID 1038860 반응식
[N+:1]([C:4]1[CH:12]=[C:11]2[C:7]([CH:8]=[N:9][N:10]2[CH2:13][O:14][CH2:15][CH2:16][Si:17]([CH3:20])([CH3:19])[CH3:18])=[CH:6][CH:5]=1)([O-])=O>CO.[Pd]>[CH3:18][Si:17]([CH3:20])([CH3:19])[CH2:16][CH2:15][O:14][CH2:13][N:10]1[C:11]2[C:7](=[CH:6][CH:5]=[C:4]([NH2:1])[CH:12]=2)[CH:8]=[N:9]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 1

HCID 534045066-Nitro-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-indazole

생성물 1

HCID 67293196HCID 67293196, 화합물수율 71.4%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

6-Nitro-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-indazole (19.2 g, 65.4 mmol) and Pd\C (10 wt %, 1.920 g) were combined in MeOH (60 mL). The mixture was allowed to stir under an atmosphere of H2 at ambient pressure and at rt for about 18 h. The mixture was filtered and the filtrate was concentrated in vacuo. The residue was purified by column chromatography (silica gel, 10:1 Hex/EtOAc) to give 1-((2-(trimethylsilyl)ethoxy)methyl)-1H-indazol-6-amine (12.3 g, 71%): LC/MS (Table 2, Method h) Rt=2.09 min; MS m/z: 264 (M+H)+.

후처리

  1. filtrationThe mixture was filtered
  2. concentrationthe filtrate was concentrated in vacuo
  3. customThe residue was purified by column chromatography (silica gel, 10:1 Hex/EtOAc)

출처 및 근거

ORD 기록
ord-39511f40b9594ecf8d7874aa75d1a427
출처 데이터셋
uspto-grants-2013_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08551981B2

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