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Nitroethane → 2-(Heptyloxy)-6-(1-nitroethyl)quinoline

HRID 709909
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HRID 709909 반응식
Br[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[N:8]=[C:7]([O:12][CH2:13][CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19])[CH:6]=[CH:5]2.[N+:20]([CH2:23][CH3:24])([O-:22])=[O:21].C(=O)([O-])[O-].[Cs+].[Cs+]>COCCOC.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C(P(C(C)(C)C)C1C=CC=CC=1C1C=CC=CC=1C)(C)(C)C>[CH2:13]([O:12][C:7]1[CH:6]=[CH:5][C:4]2[C:9](=[CH:10][CH:11]=[C:2]([CH:23]([N+:20]([O-:22])=[O:21])[CH3:24])[CH:3]=2)[N:8]=1)[CH2:14][CH2:15][CH2:16][CH2:17][CH2:18][CH3:19]
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참가 물질

7

반응물 3

HCID 6587NitroethaneHCID 10796Cesium carbonateHCID 674087426-Bromo-2-(heptyloxy)quinoline

생성물 1

HCID 866429352-(Heptyloxy)-6-(1-nitroethyl)quinoline수율 78%

시약·촉매·용매 3

HCID 27349372-(Di-tert-butylphosphino)-2'-methyl-1,1'-biphenyl촉매
HCID 9811564
Bis(dibenzylideneacetone)palladium
촉매
HCID 80711,2-Dimethoxyethane용매

실험 절차

6-bromo-2-(heptyloxy)quinoline (2.014 g, 6.27 mmol) and Pd2(dba)3 (172 mg, 0.188 mmol, 0.03 eq.) were dissolved in DME (5 mL) and stirred under nitrogen atmosphere for 10 min. 2-di-tert-butylphosphino-2′-methylbiphenyl (117 mg, 0.36 mmol, 0.06 eq.) was added and the mixture was stirred at r.t. for 10 min. Then nitroethane (0.9 mL, 12.54 mmol, 2.0 eq.) and cesium carbonate (2.5 g, 7.5 mmol, 1.2 eq.) were added. The mixture was stirred at 50° C. under nitrogen atmosphere for 15 h. The mixture was extracted with ethyl acetate and the organic layer was purified by silica gel column chromatography using petroleum/ethyl acetate (5/1) as eluent to give product as a slight red oil (1.5 g, 78%). ESI-MS: 317.1 (M+H)+. 1H NMR (400 MHz, CDCl3) δ 7.98 (d, 1H), 7.86 (d, 1H), 7.79 (s, 1H), 7.69 (q, 1H), 6.93 (d, 1H), 5.77-5.74 is (m, 1H), 4.46 (t, 2H), 1.98 (d, 3H), 1.84-1.80 (m, 2H), 1.48-1.29 (m, 8H), 0.89 (t, 3H).

후처리

  1. stirringthe mixture was stirred at r.t. for 10 min
  2. stirringThe mixture was stirred at 50° C. under nitrogen atmosphere for 15 h
  3. extractionThe mixture was extracted with ethyl acetate
  4. customthe organic layer was purified by silica gel column chromatography

출처 및 근거

ORD 기록
ord-55feb6a1c6884d7ebb865e18d18ad509
출처 데이터셋
uspto-grants-2015_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09181191B2

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