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Tetrabutylammonium Fluoride → 7-Ethynylisoindolin-1-one

HRID 1485194
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HRID 1485194 반응식
C[Si]([C:5]#[C:6][C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:15]=1[C:14](=[O:16])[NH:13][CH2:12]2)(C)C.CCCC[N+](CCCC)(CCCC)CCCC.[F-]>C1COCC1>[C:6]([C:7]1[CH:8]=[CH:9][CH:10]=[C:11]2[C:15]=1[C:14](=[O:16])[NH:13][CH2:12]2)#[CH:5]
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참가 물질

4

반응물 2

HCID 2724141Tetrabutylammonium FluorideHCID 682830087-((Trimethylsilyl)ethynyl)isoindolin-1-one

생성물 1

HCID 866757197-Ethynylisoindolin-1-one수율 76.3%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To a solution of 7-((trimethylsilyl)ethynyl)isoindolin-1-one (160) (0.172 g, 0.634 mmol) in dry THF (8 mL) under an atmosphere of nitrogen was added TBAF (1.0 M in THF, 0.697 mL, 0.697 mmol) dropwise at 0° C. The solution was stirred at this temperature for 1.5 hours and then quenched by the addition of water (2 mL). The reaction mixture was concentrated in vacuo and diluted with DCM (100 mL) and sat. aq. NaHCO3 (70 mL). The layers were separated and the aqueous layer was extracted with DCM (70 mL), the combined organic layers were washed with water (100 mL), brine (100 mL), dried (MgSO4), filtered and concentrated in vacuo to give a beige solid. The crude product was purified by silica gel chromatography (Biotage Isolera, 12 g Si Cartridge, 0-80% EtOAc in DCM) to give the title compound (I61) (0.076 g, 76% yield) as an off-white solid; 1H NMR (400 MHz, d6-DMSO) δ 8.59 (s, 1H), 7.61-7.50 (m, 3H), 4.39 (s, 1H), 4.33 (s, 2H). LCMS Method C: rt 4.56 min, m/z 158.1 [M+H]+

후처리

  1. customquenched by the addition of water (2 mL)
  2. concentrationThe reaction mixture was concentrated in vacuo
  3. additiondiluted with DCM (100 mL) and sat. aq. NaHCO3 (70 mL)
  4. customThe layers were separated
  5. extractionthe aqueous layer was extracted with DCM (70 mL)
  6. washthe combined organic layers were washed with water (100 mL), brine (100 mL)
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customto give a beige solid
  11. customThe crude product was purified by silica gel chromatography (Biotage Isolera, 12 g Si Cartridge, 0-80% EtOAc in DCM)

출처 및 근거

ORD 기록
ord-4e8ebf08faa0431a85a40b945643b09d
출처 데이터셋
uspto-grants-2016_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09421205B2

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