Reaktion #67695

Reaktionsgleichung

HCl

2-Methoxy-6-methylsulfanyl-4-trifluoromethyl-N-(1,4,8-trioxa-spiro[4.5]dec-6-yl)-benzamide

intermediate B

2-Methoxy-6-methylsulfanyl-4-trifluoromethyl-N-(1,4,8-trioxa-spiro[4.5]dec-6-yl)-benzamide

→

2-Methoxy-6-methylsulfanyl-N-(4-oxo-tetrahydro-pyran-3-yl)-4-trifluoromethyl-benzamide

Lösungsmittel

dioxane

tetrahydrofuran

water

ethyl acetate

sodium bicarbonate

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe reaction mixture was refluxed for 2 h
2. 2
   ExtraktionThe mixture was extracted two times with ethyl acetate
3. 3
   TrocknenThe combined organic layers were dried with sodium sulfate
4. 4
   Filtrationfiltered
5. 5
   Sonstigeevaporated

Vorschrift

2-Methoxy-6-methylsulfanyl-4-trifluoromethyl-N-(1,4,8-trioxa-spiro[4.5]dec-6-yl)-benzamide (intermediate B, 200 mg, 0.49 mmol) was dissolved in 1 mL tetrahydrofuran and 1 mL 4N HCl in dioxane was added. The reaction mixture was refluxed for 2 h. The mixture was diluted with water, ethyl acetate and neutralized with saturated sodium bicarbonate solution. The mixture was extracted two times with ethyl acetate. The combined organic layers were dried with sodium sulfate, filtered and evaporated. The crude product was used for the next step.

Quelle