Reaktion #219277

Reaktionsgleichung

1,4-Dioxa-spiro[4.5]decan-8-one

2-Methyl-propane-2-sulfinic acid amide

NaHCO3

→

Compound 15

Ausbeute 45.8%

2-Methyl-propane-2-sulfinic acid (1,4-dioxa-spiro[4.5]dec-8-ylidene)-amide

Ausbeute 45.8%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Sonstigeby flushing with N2(g) for 30 min
2. 2
   Filtrationfollowed by filtration
3. 3
   Waschenan EtOAc rinse
4. 4
   TrocknenThe organic layer was dried with MgSO4
5. 5
   Filtrationfiltered
6. 6
   Einengenconcentrated under reduced pressure

Vorschrift

An oven dried round-bottom flask was cooled to room temperature by flushing with N2(g) for 30 min. 1,4-Dioxa-spiro[4.5]decan-8-one (1.35 g, 8.66 mmol) (dissolved in 12 mL THF), 2-Methyl-propane-2-sulfinic acid amide (1.0 g, 8.25 mmol) (dissolved in THF), and titanium(IV) ethoxide (3.77 g, 16.50 mmol) were added. The reaction was stirred for 4 h at room temperature. To the mixture was added 15 mL saturated NaHCO3 followed by filtration and an EtOAc rinse. The organic layer was dried with MgSO4, filtered and concentrated under reduced pressure yielding 0.98 g of Compound 15.

Quelle