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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
Notes
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Reaction equation

HRID 1779167 reaction equation
[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]
ParticipantsConditionsProcedureWorkupSources & evidenceReaction notes

Participants

7

Reactant 5

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

Product 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
Yield 80%

Reagents, catalysts & solvents 1

HCID 8028TetrahydrofuranSolvent3×

Conditions

Temperature
-78 °C

Procedure

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).

Workup

  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

Sources & evidence

ORD record
ord-827dc518a41946fe91f274fd8f31ed6a
Source dataset
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
Patent number
US09266853B2

Reaction notes

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