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Acetic Acid → tert-butyl (E)-(2S,3S)-11-(2-heptyl-[1,3]dioxolan-2-yl)-2-hydroxy-3-((S)-4-isopropyl-5,5-diphenyl-2-thioxo-oxazolidine-3-carbonyl)-2-(2-methoxy-ethyl)-undec-4-enoate

HRID 1779167
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1779167
[Cl-].[Li+].[CH2:3]([C:10]1([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20]/[CH:21]=[CH:22]/[CH2:23][C:24]([N:26]2[C@@H:30]([CH:31]([CH3:33])[CH3:32])[C:29]([C:40]3[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=3)([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)[O:28][C:27]2=[S:46])=[O:25])[O:14][CH2:13][CH2:12][O:11]1)[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9].C[Si](C)(C)[N-][Si](C)(C)C.[Li+].[CH3:57][O:58][CH2:59][CH2:60][C:61](=[O:69])[C:62]([O:64][C:65]([CH3:68])([CH3:67])[CH3:66])=[O:63].C(O)(=O)C>C1COCC1>[CH2:3]([C:10]1([CH2:15][CH2:16][CH2:17][CH2:18][CH2:19][CH2:20]/[CH:21]=[CH:22]/[C@H:23]([C:24]([N:26]2[C@@H:30]([CH:31]([CH3:33])[CH3:32])[C:29]([C:34]3[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=3)([C:40]3[CH:41]=[CH:42][CH:43]=[CH:44][CH:45]=3)[O:28][C:27]2=[S:46])=[O:25])[C@@:61]([OH:69])([CH2:60][CH2:59][O:58][CH3:57])[C:62]([O:64][C:65]([CH3:66])([CH3:67])[CH3:68])=[O:63])[O:11][CH2:12][CH2:13][O:14]1)[CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH3:9]
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

7

Edukt 5

HCID 176Acetic AcidHCID 433294Lithium ChlorideHCID 2733832Lithium hexamethyldisilazaneHCID 59850503HCID 59850503, VerbindungHCID 90060040Tert-butyl 4-methoxy-2-oxobutanoate

Produkt 1

HCID 90060091
tert-butyl (E)-(2S,3S)-11-(2-heptyl-[1,3]dioxolan-2-yl)-2-hydroxy-3-((S)-4-isopropyl-5,5-diphenyl-2-thioxo-oxazolidine-3-carbonyl)-2-(2-methoxy-ethyl)-undec-4-enoate
Ausbeute 80 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel3×

Reaktionsbedingungen

Temperatur
-78 °C

Versuchsvorschrift

Lithium chloride (5.12 g, 121 mmol) was heat dried with a heat gun under reduced pressure. Under a nitrogen atmosphere, a mixture of No. 5499685 (E)-10-(2-heptyl-[1,3]dioxolan-2-yl)-1-((S)-4-isopropyl-5,5-diphenyl-2-thioxo-oxazolidin-3-yl)-dec-3-en-1-one (25.0 g, 40.3 mmol) and THF (80 mL) was added at room temperature. Further THF (145 mL) was then added to the reaction vessel. The mixture was stirred until it became homogeneous and then cooled to −78° C. Lithium hexamethyldisilazide (1 M solution in THF, 7.74 mL, 7.74 mmol) was added, and the mixture was stirred for 2 h. To the reaction mixture was added dropwise a mixture of tert-butyl 4-methoxy-2-oxo-butyrate (10.6 g, 56.5 mmol) and THF (25 mL) and the mixture was stirred for further 1 hour. To the reaction mixture was added acetic acid (4.61 mL, 80.6 mmol) and the cooling bus was removed. Water was added and the mixture was extracted with ethyl acetate. The organic layer was then washed with water, an aqueous solution of 1% NaHCO3, water, and a saturated brine in this order, and dried over anhydrous sodium sulfate. The solvent was then distilled off under reduced pressure. The resulting residue was purified with SP1 (SiO2 cartridge, 20% ethyl acetate/n-hexane, Rf=0.3) to obtain No. 6801291, tert-butyl (E)-(2S,3S)-11-(2-heptyl-[1,3]dioxolan-2-yl)-2-hydroxy-3-((S)-4-isopropyl-5,5-diphenyl-2-thioxo-oxazolidine-3-carbonyl)-2-(2-methoxy-ethyl)-undec-4-enoate (25.9 g, 80% yield).

Aufarbeitung

  1. customdried with a heat gun under reduced pressure
  2. additionUnder a nitrogen atmosphere, a mixture of No
  3. stirringthe mixture was stirred for 2 h
  4. additionTo the reaction mixture was added dropwise
  5. stirringthe mixture was stirred for further 1 hour
  6. customthe cooling bus was removed
  7. additionWater was added
  8. extractionthe mixture was extracted with ethyl acetate
  9. washThe organic layer was then washed with water
  10. dry with materialan aqueous solution of 1% NaHCO3, water, and a saturated brine in this order, and dried over anhydrous sodium sulfate
  11. distillationThe solvent was then distilled off under reduced pressure
  12. customThe resulting residue was purified with SP1 (SiO2 cartridge, 20% ethyl acetate/n-hexane, Rf=0.3)
  13. customto obtain No

Quellen und Nachweise

ORD-Eintrag
ord-827dc518a41946fe91f274fd8f31ed6a
Quelldatensatz
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US09266853B2

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