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Isopropanol → tert-Butyl (4-{(1S,2R)-1-[(4-fluorophenyl)amino]-2-({[2-(4-methoxyphenyl)-5,5-dimethyl-1,3-dioxan-2-yl]methyl}thio)-3-oxo-3-[(4S)-2-oxo-4-phenyl-1,3-oxazolidin-3-yl]propyl}phenoxy)acetate

HRID 254089
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 254089
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]2([CH2:17][S:18][CH2:19][C:20]([N:22]3[C@@H:26]([C:27]4[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=4)[CH2:25][O:24][C:23]3=[O:33])=[O:21])[O:14][CH2:13][C:12]([CH3:16])([CH3:15])[CH2:11][O:10]2)=[CH:5][CH:4]=1.[F:34][C:35]1[CH:40]=[CH:39][C:38]([N:41]=[CH:42][C:43]2[CH:57]=[CH:56][C:46]([O:47][CH2:48][C:49]([O:51][C:52]([CH3:55])([CH3:54])[CH3:53])=[O:50])=[CH:45][CH:44]=2)=[CH:37][CH:36]=1.C(N(C(C)C)C(C)C)C.C(O)(C)C>C(Cl)Cl.CC([O-])C.CC([O-])C.CC([O-])C.CC([O-])C.[Ti+4].Cl[Ti](Cl)(Cl)Cl.O>[F:34][C:35]1[CH:36]=[CH:37][C:38]([NH:41][C@@H:42]([C:43]2[CH:44]=[CH:45][C:46]([O:47][CH2:48][C:49]([O:51][C:52]([CH3:53])([CH3:54])[CH3:55])=[O:50])=[CH:56][CH:57]=2)[C@@H:19]([S:18][CH2:17][C:9]2([C:6]3[CH:5]=[CH:4][C:3]([O:2][CH3:1])=[CH:8][CH:7]=3)[O:14][CH2:13][C:12]([CH3:16])([CH3:15])[CH2:11][O:10]2)[C:20](=[O:21])[N:22]2[C@@H:26]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[CH2:25][O:24][C:23]2=[O:33])=[CH:39][CH:40]=1
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Komponenten

9

Edukt 4

HCID 3776IsopropanolHCID 81531DiisopropylethylamineHCID 66843104(4S)-3-[({[2-(4-Methoxyphenyl)-5,5-dimethyl-1,3-dioxan-2-yl]methyl}thio)acetyl]-4-phenyl-1,3-oxazolidin-2-oneHCID 86619087Tert-butyl (4-{[(4-fluorophenyl)imino]methyl}phenoxy)acetate

Produkt 1

HCID 86619089
tert-Butyl (4-{(1S,2R)-1-[(4-fluorophenyl)amino]-2-({[2-(4-methoxyphenyl)-5,5-dimethyl-1,3-dioxan-2-yl]methyl}thio)-3-oxo-3-[(4S)-2-oxo-4-phenyl-1,3-oxazolidin-3-yl]propyl}phenoxy)acetate
Ausbeute 59 %

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 11026Titanium isopropoxideKatalysatorHCID 24193Titanium TetrachlorideKatalysatorHCID 962WaterLösungsmittelHCID 6344DichloromethaneLösungsmittel4×

Reaktionsbedingungen

Temperatur
-30 °C

Versuchsvorschrift

Tetraisopropyl orthotitanate (0.31 ml, 1.06 mmol) was added to a solution of TiCl4 (1M in CH2Cl2, 3.18 ml, 3.18 mmol) in CH2Cl2 (50 ml) at 0° C. under inert atmosphere. The mixture was stirred for ten minutes. (4S)-3-[({[2-(4-Methoxyphenyl)-5,5-dimethyl-1,3-dioxan-2-yl]methyl}thio)acetyl]-4-phenyl-1,3-oxazolidin-2-one (2.00 g, 4.24 mmol) in dry CH2Cl2 (50 ml) was added dropwise over 20 minutes. The mixture was stirred for ten minutes. tert-Butyl (4-{[(4-fluorophenyl)imino]methyl}phenoxy)acetate (2.79 g, 8.48 mmol) in dry CH2Cl2 (50 ml) was added dropwise over 30 minutes. The mixture was cooled to −30° C. and stirred for 20 minutes. Ethyl diisopropyl amine (1.45 ml, 8.48 mmol) in 10 ml dry CH2Cl2 was added dropwise over ten minutes and the mixture was stirred at −30° C. for five hours. The mixture was cooled to −78° C. Isopropanol (60 ml) was added and the temperature was allowed to rise overnight. H2O (100 ml) was added and the mixture was stirred for 20 minutes and extracted twice with diethyl ether. The combined organic layers were washed with water, dried (MgSO4) and concentrated under reduced pressure. Purification by flash-chromatography (hexane:EtOAc 3:1) afforded 2.00 g (59%) of the title compound as a yellow solid. 1H-NMR (CDCl3, 200 MHz): δ 0.6 (s, 3H), 1.3 (s, 3H), 1.5 (s, 9H), 2.6-2.9 (m, 2H), 3.3-3.5 (m, 4H), 3.8 (s, 3H), 4.1-4.3 (m, 2H), 4.5 (s, 2H), 4.6-4.8 (m, 2H), 5.0-5.4 (s, broad, 1H), 5.4 (m, 1H), 5.7 (d, 1H), 6.4 (m, 2H), 6.6-6.8 (m, 4H), 6.8-7.0 (m, 4H), 7.1-7.4 (m, 7H).

Aufarbeitung

  1. stirringThe mixture was stirred for ten minutes
  2. stirringstirred for 20 minutes
  3. stirringthe mixture was stirred at −30° C. for five hours
  4. temperatureThe mixture was cooled to −78° C
  5. stirringthe mixture was stirred for 20 minutes
  6. extractionextracted twice with diethyl ether
  7. washThe combined organic layers were washed with water
  8. dry with materialdried (MgSO4)
  9. concentrationconcentrated under reduced pressure
  10. customPurification by flash-chromatography (hexane:EtOAc 3:1)

Quellen und Nachweise

ORD-Eintrag
ord-6ef8593fc0e84be2b4ad1eb3eca871c6
Quelldatensatz
uspto-grants-2011_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07871998B2

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