تفاعل #1960501

معادلة التفاعل

5,6-difluoro-3-propyl-8-(4-propylcyclohexyl)-7,8,9,10-tetrahydro-3H-benzo[f]chromene

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5,6-difluoro-3-propyl-8-(4-propylcyclohexyl)-2,3,7,8,9,10-hexahydro-1H-benzo[f]chromene

المذيبات

THF

ظروف التفاعل

المعالجة

1. 1
   ترشيحThe reaction solution is filtered
2. 2
   أخرىthe filtrate is evaporated to dryness
3. 3
   أخرىThe residue is purified by column chromatography (SiO2, n-heptane:toluene=9:1)
4. 4
   أخرىThe further purification
5. 5
   أخرىis carried out by recrystallisation from ethanol
6. 6
   أخرىgiving

الإجراء التجريبي

5.0 g (about 11.4 mmol) of 5,6-difluoro-3-propyl-8-(4-propylcyclohexyl)-7,8,9,10-tetrahydro-3H-benzo[f]chromene are hydrogenated at atmospheric pressure in THF and in the presence of Pd/C (5% of Pd). The reaction solution is filtered, and the filtrate is evaporated to dryness. The residue is purified by column chromatography (SiO2, n-heptane:toluene=9:1). The further purification is carried out by recrystallisation from ethanol, giving a 1:1 mixture of isomeric 5,6-difluoro-3-propyl-8-(4-propylcyclohexyl)-2,3,7,8,9,10-hexahydro-1H-benzo[f]chromenes (m.p. 89° C.). This can be resolved, for example, by preparative HPLC.

المصدر