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Acetic Acid → (3S,4S)-4-[(1R)-2-{(2S,4S)-1-allyloxycarbonyl-2-(2-fluoroethyloxymethyl)pyrrolidin-4-yl-thio}-1-methyl-2-oxoethyl]-3-{(1R)-1-(t-butyldimethylsilyl-oxy)ethyl}-2-azetidinone

HRID 703590
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 703590
[Si:1]([O:8][C@@H:9]([C@@H:11]1[C@@H:14]([C@@H:15]([CH3:24])[C:16](=[O:23])N2CCSC2=S)[NH:13][C:12]1=[O:25])[CH3:10])([C:4]([CH3:7])([CH3:6])[CH3:5])([CH3:3])[CH3:2].[CH2:26]([O:29][C:30]([N:32]1[CH2:36][CH:35]([SH:37])[CH2:34][CH:33]1[CH2:38][O:39][CH2:40][CH2:41][F:42])=[O:31])[CH:27]=[CH2:28].C(N(CC)CC)C.C(O)(=O)C>O1CCCC1>[CH2:26]([O:29][C:30]([N:32]1[CH2:36][C@@H:35]([S:37][C:16](=[O:23])[C@@H:15]([C@H:14]2[NH:13][C:12](=[O:25])[C@@H:11]2[C@H:9]([O:8][Si:1]([C:4]([CH3:5])([CH3:6])[CH3:7])([CH3:2])[CH3:3])[CH3:10])[CH3:24])[CH2:34][C@H:33]1[CH2:38][O:39][CH2:40][CH2:41][F:42])=[O:31])[CH:27]=[CH2:28]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 4

HCID 176Acetic AcidHCID 8471TriethylamineHCID 14071070(3S,4R)-3-[(1R)-1-(t-butyldimethylsilyloxy)ethyl]-4-{(1R)-1-methyl-2-oxo-2-(2-thioxothiazolidin-3-yl)ethyl]-2-azetidinoneHCID 190870681-Allyloxycarbonyl-2-(2-fluoroethyloxymethyl)-4-mercaptopyrrolidine

Produkt 1

HCID 86744487
(3S,4S)-4-[(1R)-2-{(2S,4S)-1-allyloxycarbonyl-2-(2-fluoroethyloxymethyl)pyrrolidin-4-yl-thio}-1-methyl-2-oxoethyl]-3-{(1R)-1-(t-butyldimethylsilyl-oxy)ethyl}-2-azetidinone
Ausbeute 42,3 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a solution of (3S,4R)-3-[(1R)-1-(t-butyldimethylsilyloxy)ethyl]- 4-{(1R)-1-methyl-2-oxo-2-(2-thioxothiazolidin-3-yl)ethyl]-2-azetidinone (3.17 g) in tetrahydrofuran (30 ml) were added 1-allyloxycarbonyl-2-(2-fluoroethyloxymethyl)-4-mercaptopyrrolidine (2.21 g) and triethylamine (1.46 ml) at 5° C., and the mixture was stirred at room temperature for 8.5 hours. Acetic acid (0.63 ml) was added to the mixture and the mixture was evaporated. The residue was dissolved in water and ethyl acetate. The organic layer was separated, washed with water, dried and evaporated. The residue was purified by chromatography on silica gel eluting with a mixture of dichloromethane and ethyl acetate (2:1 V/V) to give (3S,4S)-4-[(1R)-2-{(2S,4S)-1-allyloxycarbonyl-2-(2-fluoroethyloxymethyl)pyrrolidin-4-yl-thio}-1-methyl-2-oxoethyl]-3-{(1R)-1-(t-butyldimethylsilyl-oxy)ethyl}-2-azetidinone (1.82 g).

Aufarbeitung

  1. customthe mixture was evaporated
  2. dissolutionThe residue was dissolved in water
  3. customThe organic layer was separated
  4. washwashed with water
  5. customdried
  6. customevaporated
  7. customThe residue was purified by chromatography on silica gel eluting with a mixture of dichloromethane and ethyl acetate (2:1 V/V)

Quellen und Nachweise

ORD-Eintrag
ord-6c308863892e4e06947e8d7c752d0899
Quelldatensatz
uspto-grants-1991_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04983596

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