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Triethylamine → (S)-4-benzyl-3-[(2S,3R)-3-(4-benzyloxy-2-ethyl-phenyl)-2-ethoxy-3-hydroxy-propionyl]-oxazolidin-2-one

HRID 2215225
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HRID 2215225 반응식
[CH2:1]([C@H:8]1[CH2:12][O:11][C:10](=[O:13])[N:9]1[C:14](=[O:19])[CH2:15][O:16][CH2:17][CH3:18])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(N([CH2:25][CH3:26])CC)C.[O-]S(C(F)(F)F)(=O)=O.C([B+]CCCC)CCC.[CH2:44]([O:51][C:52]1[CH:59]=[CH:58][C:55]([CH:56]=[O:57])=[C:54](C)[CH:53]=1)[C:45]1[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=1>ClCCl>[CH2:1]([C@H:8]1[CH2:12][O:11][C:10](=[O:13])[N:9]1[C:14](=[O:19])[C@@H:15]([O:16][CH2:17][CH3:18])[C@@H:56]([C:55]1[CH:58]=[CH:59][C:52]([O:51][CH2:44][C:45]2[CH:50]=[CH:49][CH:48]=[CH:47][CH:46]=2)=[CH:53][C:54]=1[CH2:25][CH3:26])[OH:57])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1
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참가 물질

6

반응물 4

HCID 8471TriethylamineHCID 27598062-Methyl 4-benzyloxybenzaldehydeHCID 10825429(S)-4-Benzyl-3-(ethoxyacetyl)oxazolidin-2-one2회HCID 178418657HCID 178418657, 화합물

생성물 1

HCID 68616438(S)-4-benzyl-3-[(2S,3R)-3-(4-benzyloxy-2-ethyl-phenyl)-2-ethoxy-3-hydroxy-propionyl]-oxazolidin-2-one수율 58%

시약·촉매·용매

1
HCID 6344Dichloromethane용매2회

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온도
-78 °C

실험 절차

(S)-4-Benzyl-3-ethoxyacetyl-oxazolidin-2-one (6.21 g, 24 mmol) (for the preparation of (S)-4-benzyl-3-ethoxyacetyl-oxazolidin-2-one see: D. Haigh, H. C. Birrell, B. C. C. Cantello, D. S. Eggleston, R. C. Haltiwanger, R. M. Hindley, A. Ramaswamy, N. C. Stevens, Tetrahedron: Asymmetry 1999, 10, 1353–1367) was dissolved in dry dichloromethane (135 ml) under an argon atmosphere and the solution was cooled to −78° C. Triethylamine (3.98 ml, 28 mmol) was added, followed by the slow addition, over approximately 20 min, of di-n-butylboron triflate (1 M solution in dichloromethane, 25 ml, 25 mmol) such that the reaction temperature was kept below −70° C. The mixture was stirred at −78° C. for 50 min, the cooling bath was replaced with an ice bath and the mixture stirred at 0° C. for additional 50 min before being recooled to −78° C. A solution of 4-benzyloxy-2-methyl-benzaldehyde (6 g, 24 mmol) in dry dichloromethane (65 ml) was added over ca. 45 min, such that the reaction temperature was maintained below −70° C. The resulting mixture was stirred at −78° C. for 45 min, warmed from −78° C. to 0° C. and stirred at 0° C. for a further 1.5 h. The reaction mixture was poured onto ice water/brine and extracted two times with dichloromethane. The combined extracts were washed with brine and dried over sodium sulfate. The solvent was removed under reduced pressure and the residue purified by column chromatography (silica gel, cyclohexane/AcOEt) to give 6.9 g (13.7 mmol, 58%) of the title compound as yellow foam. According to 1H-NMR spectroscopy, one of the four isomers is strongly predominating. The configuration was tentatively assigned as 2S,3R according to D. Haigh et al., Tetrahedron: Asymmetry 1999, 10, 1353–1367.

후처리

  1. customwas kept below −70° C
  2. customthe cooling bath was replaced with an ice bath
  3. stirringthe mixture stirred at 0° C. for additional 50 min
  4. custombefore being recooled to −78° C
  5. temperaturewas maintained below −70° C
  6. stirringThe resulting mixture was stirred at −78° C. for 45 min
  7. temperaturewarmed from −78° C. to 0° C.
  8. stirringstirred at 0° C. for a further 1.5 h
  9. additionThe reaction mixture was poured onto ice water/brine
  10. extractionextracted two times with dichloromethane
  11. washThe combined extracts were washed with brine
  12. dry with materialdried over sodium sulfate
  13. customThe solvent was removed under reduced pressure
  14. customthe residue purified by column chromatography (silica gel, cyclohexane/AcOEt)

출처 및 근거

ORD 기록
ord-5cc14a9198454df1ab19031d1f1675ea
출처 데이터셋
uspto-grants-2006_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07109225B2

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