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Potassium Carbonate → 4,6-difluoro-5-[4-(1-hydroxy-2-methylpropan-2-yl)phenyl]-1H-indole-3-carbaldehyde

HRID 1054635
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HRID 1054635 반응식
CC1(C)COB([C:8]2[CH:13]=[CH:12][C:11]([C:14]([CH3:18])([CH3:17])[CH2:15][OH:16])=[CH:10][CH:9]=2)OC1.Br[C:21]1[C:22]([F:33])=[C:23]2[C:27](=[CH:28][C:29]=1[F:30])[NH:26][CH:25]=[C:24]2[CH:31]=[O:32].C(=O)([O-])[O-].[K+].[K+]>C1(C)C=CC=CC=1.CCO.O.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[F:33][C:22]1[C:21]([C:8]2[CH:9]=[CH:10][C:11]([C:14]([CH3:17])([CH3:18])[CH2:15][OH:16])=[CH:12][CH:13]=2)=[C:29]([F:30])[CH:28]=[C:27]2[C:23]=1[C:24]([CH:31]=[O:32])=[CH:25][NH:26]2
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참가 물질

8

반응물 3

HCID 11430Potassium CarbonateHCID 866985785-Bromo-4,6-difluoro-1H-indole-3-carbaldehydeHCID 866986392-(4-(5,5-Dimethyl-1,3,2-dioxaborinan-2-yl)phenyl)-2-methylpropan-1-ol

생성물 1

HCID 866986404,6-difluoro-5-[4-(1-hydroxy-2-methylpropan-2-yl)phenyl]-1H-indole-3-carbaldehyde수율 32%

시약·촉매·용매 4

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
촉매
HCID 702Ethanol용매
HCID 962Water용매
HCID 1140Toluene용매

실험 절차

To a solution of 2-[4-(5,5-dimethyl-1,3,2-dioxaborinan-2-yl)phenyl]-2-methylpropan-1-ol (102 mg, 0.386 mmol) and 5-bromo-4,6-difluoro-1H-indole-3-carbaldehyde (100 mg, 0.386 mmol) in toluene (6 mL) and EtOH (2 mL) was added a solution of potassium carbonate (160 mg, 1.159 mmol) in water (1.0 mL) and Pd(dppf)Cl2 (15.8 mg, 0.019 mmol) at room temperature under N2. The reaction was cooled to room temperature, and extracted with ethyl acetate (10 mL×2). The organic layers were washed with brine (10 mL), and dried over sodium sulfate and concentrated to give a crude residue, which was purified by column chromatography to give the title compound (40 mg, 32%) as a yellow solid. 1H NMR (400 MHz, CD3OD) δ 10.0 (s, 1 H), 8.13 (s, 1 H), 7.51 (d, 2 H), 7.40 (d, 2 H), 7.19 (d, 1 H), 3.63 (s, 2 H), 1.36 (s, 6 H).

후처리

  1. extractionextracted with ethyl acetate (10 mL×2)
  2. washThe organic layers were washed with brine (10 mL)
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated
  5. customto give a crude residue, which
  6. customwas purified by column chromatography

출처 및 근거

ORD 기록
ord-75cd2b174edc49e4baa40e7cd6f64bef
출처 데이터셋
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09394285B2

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