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Water → tert-Butyl 2-(6-formylpyridin-2-yl)benzyl(phenyl)carbamate

HRID 1188303
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HRID 1188303 반응식
O.C(=O)([O-])[O-].[Na+].[Na+].Br[C:9]1[N:14]=[C:13]([CH:15]=[O:16])[CH:12]=[CH:11][CH:10]=1.[C:17]1([N:23]([CH2:31][C:32]2[CH:37]=[CH:36][CH:35]=[CH:34][C:33]=2B2OC(C)(C)C(C)(C)O2)[C:24](=[O:30])[O:25][C:26]([CH3:29])([CH3:28])[CH3:27])[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>C1(C)C=CC=CC=1.O.CO.CO>[CH:15]([C:13]1[N:14]=[C:9]([C:33]2[CH:34]=[CH:35][CH:36]=[CH:37][C:32]=2[CH2:31][N:23]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[C:24](=[O:30])[O:25][C:26]([CH3:29])([CH3:28])[CH3:27])[CH:10]=[CH:11][CH:12]=1)=[O:16]
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8

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HCID 962WaterHCID 10340Sodium CarbonateHCID 27570096-Bromopyridine-2-carbaldehydeHCID 66795645Tert-butyl phenyl(2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzyl)carbamate

생성물 1

HCID 58434438tert-Butyl 2-(6-formylpyridin-2-yl)benzyl(phenyl)carbamate수율 840%

시약·촉매·용매 3

HCID 887
Methanol
용매
HCID 1140Toluene용매2회
HCID 22242641Methanol--water (1/1)용매

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온도
80 °C

실험 절차

A mixture of water (160 mL) and methanol (40 mL) was combined with sodium carbonate (3.80 g, 35.9 mmol), and the mixture was sparged with nitrogen for 30 min. In a separate flask were combined, under nitrogen, 6-bromo-2-pyridinecarboxaldehyde (2.67 g, 14.4 mmol), tert-butyl phenyl(2-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)benzyl)carbamate (5.87 g, 14.4 mmol), tetrakis(triphenylphosphinio)palladium (0.829 g, 0.718 mmol), and toluene (150 mL). The water-methanol solution was added via cannula to the toluene solution, and the biphasic mixture was heated to 80° C. overnight. At this time 1H NMR spectroscopic analysis of an aliquot indicated that the reaction was complete. The clear yellow organic layer was separated, dried with brine, then over magnesium sulfate. The crude product was purified by chromatography on silica using 1:1 hexanes:dichloromethane elutant and increasing the strength by addition of up to 10% EtOAc. The product was isolated as a sticky oil (4.7 g, 840%). 1H NMR (CD2Cl2, 500 MHz): 10.0 (s, 1H), 7.83-7.92 (m, 2H), 7.56 (d, 1H), 7.50 (d, 1H), 7.44 (m, 1H), 7.36 (m, 2H), 7.17 (t, 2H), 7.01 (t, 1H), 7.0 (br d, 2H), 5.11 (s, 2H), 1.34 (s, 9H).

후처리

  1. customthe mixture was sparged with nitrogen for 30 min
  2. customIn a separate flask were combined, under nitrogen
  3. customThe clear yellow organic layer was separated
  4. dry with materialdried with brine
  5. customThe crude product was purified by chromatography on silica using 1:1 hexanes
  6. temperaturedichloromethane elutant and increasing the strength
  7. additionby addition of up to 10% EtOAc

출처 및 근거

ORD 기록
ord-f50792b32f6d43798993db0a2cc077e1
출처 데이터셋
uspto-grants-2014_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08674040B2

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