تفاعل #1687670

معادلة التفاعل

benzyl 2-hydroxy-3-[2-methyl-3-[1,3,3,3-tetramethyl-1-[(trimethylsilyl)oxy]disiloxanyl]propyl]benzoate

cyclohexene

→

2-hydroxy-3-[2-methyl-3-[1,3,3,3-tetramethyl-1-[(trimethylsilyl)oxy]disiloxanyl]-propyl]benzoic acid

المردود 78.6%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةwas maintained
2. 2
   درجة الحرارةat reflux for 1 hour
3. 3
   درجة الحرارةThe mixture was cooled
4. 4
   غسيلrinsed with ethanol
5. 5
   تركيزThe liquids were concentrated
6. 6
   أخرىthe pale yellow oil obtained
7. 7
   أخرىwas purified by chromatography on silica under pressure (eluent: 80/20/0.2 CH2Cl2 /ethyl acetate/acetic acid)

الإجراء التجريبي

A mixture of the above crude oil of benzyl 2-hydroxy-3-[2-methyl-3-[1,3,3,3-tetramethyl-1-[(trimethylsilyl)oxy]disiloxanyl]propyl]benzoate (11.61 g, 0.023 mol), ethanol (40 ml), cyclohexene (12 ml) and 10% palladium-on-charcoal (1.2 g) was maintained at reflux for 1 hour. The mixture was cooled and rinsed with ethanol. The liquids were concentrated and the pale yellow oil obtained was purified by chromatography on silica under pressure (eluent: 80/20/0.2 CH2Cl2 /ethyl acetate/acetic acid) to give 7.5 g (yield: 78%) of 2-hydroxy-3-[2-methyl-3-[1,3,3,3-tetramethyl-1-[(trimethylsilyl)oxy]disiloxanyl]-propyl]benzoic acid in the form of a colourless oil.

المصدر