تفاعل #2482733

معادلة التفاعل

4-(3-cyclopropyl-2-t-butyloxycarbonyl-1,3-dioxoprop-1-yl)-2,2-difluoro-7-methylsulphenyl-1,3-benzodioxole

para-toluenesulphonic acid

→

4-(3-cyclopropyl-1,3-dioxoprop-1-yl)-2,2-difluoro-7-methylsulphenyl-1,3-benzodioxole

المردود 84.6%

المذيبات

toluene

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةAfter cooling
2. 2
   أخرىthe solvent was evaporated in vacuo, and ethyl acetate
3. 3
   workup.ADDITIONadded
4. 4
   غسيلThe solution was washed with water
5. 5
   تجفيفdried over anhydrous magnesium sulphate
6. 6
   أخرىevaporated
7. 7
   أخرىThe residue was purified by column chromatography
8. 8
   غسيلeluting with ethyl acetate/cyclohexane

الإجراء التجريبي

A solution of 4-(3-cyclopropyl-2-t-butyloxycarbonyl-1,3-dioxoprop-1-yl)-2,2-difluoro-7-methylsulphenyl-1,3-benzodioxole (10.3 g) and para-toluenesulphonic acid (0.5 g) was heated under reflux with toluene for 3 hours. After cooling, the solvent was evaporated in vacuo, and ethyl acetate added. The solution was washed with water, dried over anhydrous magnesium sulphate and evaporated. The residue was purified by column chromatography, eluting with ethyl acetate/cyclohexane to yield 4-(3-cyclopropyl-1,3-dioxoprop-1-yl)-2,2-difluoro-7-methylsulphenyl-1,3-benzodioxole (6.61 g) m.p. 117.5°-118.5° C.

المصدر