반응 #67695

반응 방정식

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

용매

dioxane

tetrahydrofuran

water

ethyl acetate

sodium bicarbonate

반응 조건

후처리

1. 1
   온도The reaction mixture was refluxed for 2 h
2. 2
   추출The mixture was extracted two times with ethyl acetate
3. 3
   건조The combined organic layers were dried with sodium sulfate
4. 4
   여과filtered
5. 5
   기타evaporated

실험 절차

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.

출처