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Tributyltin iodide → 1-cyclobutyl-6-difluoromethoxy-2-tributylstannanyl-1H-indole-3-carbonitrile

HRID 1028000
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HRID 1028000 반응식
[CH:1]1([N:5]2[C:13]3[C:8](=[CH:9][CH:10]=[C:11]([O:14][CH:15]([F:17])[F:16])[CH:12]=3)[C:7]([C:18]#[N:19])=[CH:6]2)[CH2:4][CH2:3][CH2:2]1.[CH2:20]([Sn:24](I)([CH2:29][CH2:30][CH2:31][CH3:32])[CH2:25][CH2:26][CH2:27][CH3:28])[CH2:21][CH2:22][CH3:23].[Li+].CC([N-]C(C)C)C>C1COCC1>[CH:1]1([N:5]2[C:13]3[C:8](=[CH:9][CH:10]=[C:11]([O:14][CH:15]([F:16])[F:17])[CH:12]=3)[C:7]([C:18]#[N:19])=[C:6]2[Sn:24]([CH2:25][CH2:26][CH2:27][CH3:28])([CH2:29][CH2:30][CH2:31][CH3:32])[CH2:20][CH2:21][CH2:22][CH3:23])[CH2:2][CH2:3][CH2:4]1
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참가 물질

5

반응물 3

HCID 23765Tributyltin iodideHCID 2724682Lithium diisopropylamideHCID 667306391-cyclobutyl-6-(difluoromethoxy)-1H-indole-3-carbonitrile

생성물 1

HCID 667305741-cyclobutyl-6-difluoromethoxy-2-tributylstannanyl-1H-indole-3-carbonitrile

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
-78 °C

실험 절차

To 1-cyclobutyl-6-difluoromethoxy-1H-indole-3-carbonitrile (830 mg, 3.17 mmol) in THF (10 mL) was added tributyltin iodide (1.13 mL, 4.04 mmol) and the solution cooled to −78° C. A solution of LDA (1.5M in cyclohexane, 3.4 mL, 5.1 mmol) was added dropwise. After complete addition the bath was removed and the mixture stirred at room temperature for 1 hour. THF was then removed under vacuum and the residue filtered through silica gel using CH2Cl2 as an eluant and the mixture concentrated. The residue was purified by flash chromatography using 30-50% CH2Cl2/hexanes to provide 1-cyclobutyl-6-difluoromethoxy-2-tributylstannanyl-1H-indole-3-carbonitrile as a clear, colorless oil (1.23 g, 70%).

후처리

  1. additionAfter complete addition the bath
  2. customwas removed
  3. customTHF was then removed under vacuum
  4. filtrationthe residue filtered through silica gel
  5. concentrationthe mixture concentrated
  6. customThe residue was purified by flash chromatography

출처 및 근거

ORD 기록
ord-6204be65cd7e449f9062b60d63186818
출처 데이터셋
uspto-grants-2014_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08735414B2

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