반응 #11787

반응 방정식

2-(5-chloro-2-methoxy-phenylsulfanyl)-2-methyl-propionic acid methyl ester

hydrobromic acid

→

title compound

6-Chloro-3,3-dimethyl-benzo[1,4]oxathiin-2-one

반응 조건

후처리

1. 1
   온도The reaction was heated
2. 2
   온도to reflux for 24 hours at which time the solvent
3. 3
   기타was removed by evaporation
4. 4
   workup.ADDITIONTo the crude acid phenol was added toluene (5 ml) and catalytic pyridinium p-toluenesulfonate
5. 5
   온도After 12 hours of heating
6. 6
   온도at reflux the reaction
7. 7
   농축was concentrated

실험 절차

To 2-(5-chloro-2-methoxy-phenylsulfanyl)-2-methyl-propionic acid methyl ester (prepared from 5-chloro-2-methoxy-benzenesulfonyl chloride: Syn. Comm., (2001), 31, 505–510) (0.25 g, 0.9 mmol) was added 48% hydrobromic acid (5 ml). The reaction was heated to reflux for 24 hours at which time the solvent was removed by evaporation. To the crude acid phenol was added toluene (5 ml) and catalytic pyridinium p-toluenesulfonate. After 12 hours of heating at reflux the reaction was concentrated and the title compound was isolated by chromatography on silica gel (0.27 g).

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