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Citric Acid → (S)-2-(tert-butyldimethylsilyloxy)-3-isopropoxy-N-(5-(methylthio)pyridin-2-yl)propanamide

HRID 1098197
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1098197
C[Al](C)C.[CH3:5][S:6][C:7]1[CH:8]=[CH:9][C:10]([NH2:13])=[N:11][CH:12]=1.[Si:14]([O:21][C@@H:22]([CH2:27][O:28][CH:29]([CH3:31])[CH3:30])[C:23](OC)=[O:24])([C:17]([CH3:20])([CH3:19])[CH3:18])([CH3:16])[CH3:15].C(O)(=O)CC(CC(O)=O)(C(O)=O)O>C1(C)C=CC=CC=1.O.CCOC(C)=O>[Si:14]([O:21][C@@H:22]([CH2:27][O:28][CH:29]([CH3:31])[CH3:30])[C:23]([NH:13][C:10]1[CH:9]=[CH:8][C:7]([S:6][CH3:5])=[CH:12][N:11]=1)=[O:24])([C:17]([CH3:20])([CH3:19])[CH3:18])([CH3:16])[CH3:15]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

8

Edukt 4

HCID 311Citric AcidHCID 151797975-(Methylsulfanyl)pyridin-2-amineHCID 16682925TrimethylaluminumHCID 59279534(S)-methyl 2-(tert-butyldimethylsilyloxy)-3-isopropoxypropanoate

Produkt 1

HCID 57504670(S)-2-(tert-butyldimethylsilyloxy)-3-isopropoxy-N-(5-(methylthio)pyridin-2-yl)propanamideAusbeute 56,8 %

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 1140TolueneLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
0 °C

Versuchsvorschrift

Trimethylaluminium (2M in toluene) (10.40 mL, 20.80 mmol) was added to 5-(methylthio)pyridin-2-amine (CAS no. 77618-99-6) (2.54 g, 18.09 mmol) in toluene (100 mL) cooled to 0° C. under nitrogen. The resulting solution was stirred at 0° C. for 20 minutes. (S)-methyl 2-(tert-butyldimethylsilyloxy)-3-isopropoxypropanoate (Intermediate C7b) (5 g, 18.09 mmol) was added and the reaction was allowed to warm to room temperature. The reaction was allowed to stir at room temperature for 1 hour. The temperature was increased to 60° C. and stirred for a further 24 hours. The reaction mixture was neutralised with citric acid (1M, aq) and then diluted with water and EtOAc (200 mL). The organic layer was separated and the aqueous layer re-extracted with EtOAc (100 mL). The combined organics were dried (MgSO4), filtered and evaporated in vacuo. The crude product was purified by flash silica chromatography, elution gradient 0 to 50% Et2O in isohexane to afford the product (3.95 g, 56.8%). 1H NMR (400 MHz, DMSO) δ 0.10-0.13 (6H, d), 0.90-0.92 (9H, m), 1.04-1.07 (6H, m), 2.40 (3H +DMSO, s), 3.54-3.63 (3H, m), 4.42-4.44 (1H, m), 7.77-7.80 (1H, dd), 8.03-8.06 (1H, d), 8.26 (1H, d), 9.49 (1H, s); m/z (ES+) (M+H)+=385; HPLC tR=3.66 min.

Aufarbeitung

  1. temperatureto warm to room temperature
  2. stirringto stir at room temperature for 1 hour
  3. temperatureThe temperature was increased to 60° C.
  4. stirringstirred for a further 24 hours
  5. customThe organic layer was separated
  6. extractionthe aqueous layer re-extracted with EtOAc (100 mL)
  7. dry with materialThe combined organics were dried (MgSO4)
  8. filtrationfiltered
  9. customevaporated in vacuo
  10. customThe crude product was purified by flash silica chromatography, elution gradient 0 to 50% Et2O in isohexane

Quellen und Nachweise

ORD-Eintrag
ord-95c246d54882428d9c1789548abb1259
Quelldatensatz
uspto-grants-2012_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08143263B2

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