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Acetic Acid → (S)-methyl 2-(tert-butyldiphenylsilyloxy)-4-(methylthio)butanoate

HRID 1098165
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1098165
[CH3:1][Si](C=[N+]=[N-])(C)C.CO.[Si:10]([O:27][C@@H:28]([CH2:32][CH2:33][S:34][CH3:35])[C:29]([OH:31])=[O:30])([C:23]([CH3:26])([CH3:25])[CH3:24])([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:11]1[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=1.C(O)(=O)C>C1(C)C=CC=CC=1>[Si:10]([O:27][C@@H:28]([CH2:32][CH2:33][S:34][CH3:35])[C:29]([O:31][CH3:1])=[O:30])([C:23]([CH3:26])([CH3:25])[CH3:24])([C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1)[C:11]1[CH:12]=[CH:13][CH:14]=[CH:15][CH:16]=1
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Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 887MethanolHCID 167693TrimethylsilyldiazomethaneHCID 57504643(S)-2-(tert-butyldiphenylsilyloxy)-4-(methylthio)butanoic acid

Produkt 1

HCID 66813184(S)-methyl 2-(tert-butyldiphenylsilyloxy)-4-(methylthio)butanoateAusbeute 72,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1140TolueneLösungsmittel

Versuchsvorschrift

Sodium thiomethoxide (0.187 g, 2.67 mmol) was added to (S)-3-(tert-butyldiphenylsilyloxy)dihydrofuran-2(3H)-one (CAS no. 220351-82-6: Klar, U.; Schwede, W.; Skuballa, W.; Buchmann, B.; Schirner, M. Ger. Offen. 1999 DE 19735575 A1) (0.826 g, 2.43 mmol) in DMF (2 mL) at 0° C. The resulting solution was stirred at room temperature for 16 hours. The reaction mixture was neutralised with 2M HCl and diluted with ethyl acetate. The organic layer was extracted with water (3×100 mL), the organic layer was dried (MgSO4) and evaporated to afford (S)-2-(tert-butyldiphenylsilyloxy)-4-(methylthio)butanoic acid (0.160 g, 16.98%) which was used without further purification. A solution of trimethylsilyldiazomethane (2M solution in ether, 0.412 ml, 0.82 mmol) was added dropwise to a stirred solution of methyl alcohol (0.167 ml, 4.12 mmol) and (S)-2-(tert-butyldiphenylsilyloxy)-4-(methylthio)butanoic acid (0.160 g, 0.41 mmol) in toluene (0.174 ml) over a period of 2 minutes. The resulting solution was stirred at ambient temperature for 2 hours. The reaction mixture was quenched with acetic acid (0.071 ml, 1.24 mmol) and stirred at ambient temperature for 10 minutes. The reaction mixture was evaporated. The residue was purified by flash silica chromatography, eluting with 0 to 50% ethyl acetate in isohexane to afford the product (0.120 g, 72.4%). 1H NMR (400 MHz, CDCl3) δ 1.09 (9H, s), 1.94-2.05 (5H, m), 2.48-2.60 (2H, m), 3.47 (3H, s), 4.33-4.36 (1H, m), 7.34-7.45 (6H, m), 7.62-7.67 (4H, m); m/z (ES+) (M-Ph)-=325; HPLC tR=3.63 min

Aufarbeitung

  1. customwas used without further purification
  2. stirringstirred at ambient temperature for 10 minutes
  3. customThe reaction mixture was evaporated
  4. customThe residue was purified by flash silica chromatography
  5. washeluting with 0 to 50% ethyl acetate in isohexane

Quellen und Nachweise

ORD-Eintrag
ord-20900d253972480b8899fa7c90d3ff24
Quelldatensatz
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08143263B2

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