تفاعل #11787

معادلة التفاعل

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

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe reaction was heated
2. 2
   درجة الحرارةto reflux for 24 hours at which time the solvent
3. 3
   أخرىwas removed by evaporation
4. 4
   workup.ADDITIONTo the crude acid phenol was added toluene (5 ml) and catalytic pyridinium p-toluenesulfonate
5. 5
   درجة الحرارةAfter 12 hours of heating
6. 6
   درجة الحرارةat reflux the reaction
7. 7
   تركيزwas concentrated

الإجراء التجريبي

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).

المصدر