Reaktion #714371

ord-2ae5512d9f3045a6829cdd18e4830b2c

Reaktionsgleichung

O=C([O-])N1CC=CCC1
5,6-dihydropyridine-1(2H)-carboxylate
CC(C)(C)OC(=O)N1CC(=O)C(CO)=C[C@H]1CO[Si](C)(C)C(C)(C)C
Intermediate 117
CC(C)(C)OC(=O)N1CC(=O)C(CO)=C[C@H]1CO[Si](C)(C)C(C)(C)C
(S)-tert-butyl 2-((tert-butyldimethylsilyloxy)methyl)-4-(hydroxymethyl)-5-oxo-5,6-dihydropyridine-1(2H)-carboxylate
COc1ccc(COC(=N)C(Cl)(Cl)Cl)cc1
4-methoxybenzyl 2,2,2-trichloroacetimidate
O=S(=O)([O-])C(F)(F)F.O=S(=O)([O-])C(F)(F)F.O=S(=O)([O-])C(F)(F)F.[La+3]
La(OTf)3
COc1ccc(COCC2=C[C@@H](CO[Si](C)(C)C(C)(C)C)N(C(=O)OC(C)(C)C)CC2=O)cc1
crude product
COc1ccc(COCC2=C[C@@H](CO[Si](C)(C)C(C)(C)C)N(C(=O)OC(C)(C)C)CC2=O)cc1
(S)-tert-butyl 2-(((tert-butyldimethylsilyl)oxy)methyl)-4-(((4-methoxybenzyl)-oxy)methyl)-5-oxo-5,6-dihydropyridine-1(2H)-carboxylate

Lösungsmittel

Reaktionsbedingungen

Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    TrocknenAqueous work-up with ethyl acetate and the organic layer was dried over MgSO4

Vorschrift

To a solution of (2S)-tert-butyl 5-hydroxy-4-(hydroxymethyl)-2-(isopropyldimethylsilyl)oxy)methyl)-5,6-dihydropyridine-1(2H)-carboxylate (Intermediate 117, 13.0 g, 34.99 mmol) in toluene (150 mL) was added 4-methoxybenzyl 2,2,2-trichloroacetimidate (7.65 mL, 10.42 g, 36.74 mmol) and La(OTf)3 (205 mg, 0.35 mmol). The mixture was stirred at 50° C. for 4 h. Aqueous work-up with ethyl acetate and the organic layer was dried over MgSO4 to afford the crude product.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US09309245B2uspto-grants-2016_04