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2-[2-[[(1,1-Dimethylethyl)diphenylsilyl]oxy]ethoxy]-5-nitropyridine → HCID 19756412, 화합물

HRID 1587825
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HRID 1587825 반응식
[Si:1]([O:18][CH2:19][CH2:20][O:21][C:22]1[CH:27]=[CH:26][C:25]([N+:28]([O-])=O)=[CH:24][N:23]=1)([C:14]([CH3:17])([CH3:16])[CH3:15])([C:8]1[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[H][H]>CO.[Pd]>[NH2:28][C:25]1[CH:26]=[CH:27][C:22]([O:21][CH2:20][CH2:19][O:18][Si:1]([C:14]([CH3:17])([CH3:16])[CH3:15])([C:2]2[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=2)[C:8]2[CH:13]=[CH:12][CH:11]=[CH:10][CH:9]=2)=[N:23][CH:24]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 197564132-[2-[[(1,1-Dimethylethyl)diphenylsilyl]oxy]ethoxy]-5-nitropyridineHCID 178418361HCID 178418361, 화합물

생성물 1

HCID 19756412HCID 19756412, 화합물수율 100.9%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 887Methanol용매

실험 절차

Compound B (106 g) was dissolved in methanol (1.35 l) and hydrogenated at atmospheric pressure over 10% palladium on charcoal catalyst (10.6 g). When hydrogen uptake was complete, the catalyst was removed by filtration through diatomaceous earth. Volatile material was then removed from the filtrate by evaporation to give 5-amino-2-[2-(t-butyldiphenylsilyl)oxyethoxy]pyridine (C) (99.4 g), as an oil which was used without further purification; NMR (d6 -DMSO): 0.95(s,9H), 3.9(t,2H), 4.25(t,2H), 4.7(brs,2H), 6.5(d,1H), 7.0(dd,1H), 7.35-7.75 (complex m,7H), 7.6-7.75(m,4H).

후처리

  1. customthe catalyst was removed by filtration through diatomaceous earth
  2. customVolatile material was then removed from the filtrate by evaporation

출처 및 근거

ORD 기록
ord-a8c3fda242c744a6834b25ab2199f53f
출처 데이터셋
uspto-grants-1993_06
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05219863

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