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Triethylamine → HCID 11774823, 화합물

HRID 625892
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HRID 625892 반응식
[C:1]([O:5][C:6]([N:8]1[C:16]2[C:11](=[CH:12][CH:13]=[CH:14][CH:15]=2)[C:10](/[CH:17]=[CH:18]/[C:19]([OH:21])=O)=[CH:9]1)=[O:7])([CH3:4])([CH3:3])[CH3:2].CCN(CC)CC.C(Cl)(=O)C(C)(C)C.C([Li])CCC.[Li].[C:42]1([C@@H:48]2[CH2:52][O:51][C:50](=[O:53])[NH:49]2)[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=1>C1COCC1>[O:21]=[C:19]([N:49]1[C@H:48]([C:42]2[CH:47]=[CH:46][CH:45]=[CH:44][CH:43]=2)[CH2:52][O:51][C:50]1=[O:53])/[CH:18]=[CH:17]/[C:10]1[C:11]2[C:16](=[CH:15][CH:14]=[CH:13][CH:12]=2)[N:8]([C:6]([O:5][C:1]([CH3:2])([CH3:4])[CH3:3])=[O:7])[CH:9]=1
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참가 물질

8

반응물 6

HCID 8471TriethylamineHCID 62493Pivaloyl chlorideHCID 730425(4R)-4-phenyl-1,3-oxazolidin-2-one2회HCID 3028194LithiumHCID 11323657HCID 11323657, 화합물HCID 178418339Butyllithium2회

생성물 1

HCID 11774823
HCID 11774823, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

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온도
-78 °C

실험 절차

To a solution of (E)-3-(1-(tert-butoxycarbonyl)-1H-indol-3-yl)acrylic acid (7.14 g, 24.85 mmol) in THF (400 mL) at −78° C. were added Et3N (10.39 ml, 74.6 mmol) and pivaloyl chloride (6.12 ml, 49.7 mmol). The mixture was stirred for 15 min at −78° C. then warmed to 0° C. for 1.5 h. The mixture was cooled to −78° C., to which was added n-Butyllithium (1.6 M in Hexanes)(14 mL, 22.4 mmol), then added the lithium salt of (R)-4-phenyl-2-oxazolidinone [prepared by adding n-Butyllithium (1.6 M in Hexanes)(31 ml, 49.7 mmol), to a solution of (R)-4-phenyloxazolidin-2-one (8.11 g, 49.7 mmol)] in THF (200 mL) at −78° C.) via cannula. The reaction was stirred at −78° C. for 2 h then at rt for 16 h. The reaction was quenched with saturated NH4Cl aqueous solution. The organics were removed under vacuum and the aqueous was extracted with EtOAc. The organic layer was collected, washed with brine, dried over sodium sulfate, and concentrated under vacuum. The crude product was purified by silica gel chromatography using a gradient of 10-20% EtOAc/Hexanes. The product fractions were collected and the solvent removed under vacuum to give ((R,E)-tert-butyl 3-(3-oxo-3-(2-oxo-4-phenyloxazolidin-3-yl)prop-1-en-1-yl)-1H-indole-1-carboxylate, 7.12 g (66%). ESI-MS (+) m/z 433.4 (M+1).

후처리

  1. temperaturethen warmed to 0° C. for 1.5 h
  2. temperatureThe mixture was cooled to −78° C., to which
  3. customprepared
  4. customat −78° C.
  5. stirringThe reaction was stirred at −78° C. for 2 h
  6. waitat rt for 16 h
  7. customThe reaction was quenched with saturated NH4Cl aqueous solution
  8. customThe organics were removed under vacuum
  9. extractionthe aqueous was extracted with EtOAc
  10. customThe organic layer was collected
  11. washwashed with brine
  12. dry with materialdried over sodium sulfate
  13. concentrationconcentrated under vacuum
  14. customThe crude product was purified by silica gel chromatography
  15. customThe product fractions were collected
  16. customthe solvent removed under vacuum

출처 및 근거

ORD 기록
ord-0c8341bb7dc848498150d67cc2ec12db
출처 데이터셋
uspto-grants-2016_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09308236B2

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