تفاعل #1047

معادلة التفاعل

methanol

compound ( 3 )

4-(4-phenoxyphenyl)-1,2,3,6-tetrahydropyridine

→

compound ( 4 )

المردود 66.0%

4-(4-phenoxyphenyl)piperidine

المردود 66.0%

المذيبات

acetic acid

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter the end of the reaction
2. 2
   ترشيحthe insolubles were filtered off
3. 3
   تركيزthe filtrate was concentrated under reduced pressure
4. 4
   workup.DISSOLUTIONThe obtained residue was dissolved in methylene chloride
5. 5
   أخرىThe organic layer was dried
6. 6
   ترشيحfiltered
7. 7
   تركيزconcentrated under reduced pressure
8. 8
   أخرىto obtain a residue which
9. 9
   أخرىwas then purified by silica gel column chromatography (methylene chloride:methanol=20:1!)

الإجراء التجريبي

To a 100 ml methanol solution of 3.51 g of the compound (3) synthesized in Reference Example 3 were added 200 mg of palladium carbon and 1 ml of acetic acid for hydrogenation at atmospheric pressure and room temperature. After the end of the reaction, the insolubles were filtered off and the filtrate was concentrated under reduced pressure. The obtained residue was dissolved in methylene chloride, then adjusted by a 10% aqueous solution of sodium hydroxide to pH=9 to 10, then was shaken. The organic layer was dried, filtered, then concentrated under reduced pressure to obtain a residue which was then purified by silica gel column chromatography (methylene chloride:methanol=20:1!) to obtain the above-reference compound (4) in all amount of 2.32 g (yield of 66%).

المصدر