تفاعل #1328402

معادلة التفاعل

N,N-dibenzyl-(1R,2S,4S)-1-methyl-2-hydroxy-4-phenylhexyl amine

acetic acid

→

(1R,2S,4S)-1-methyl-2-hydroxy-4-phenylhexyl amine

المردود 78.5%

المذيبات

methanol

ظروف التفاعل

المعالجة

1. 1
   ترشيحthe catalyst was filtered off
2. 2
   أخرىThe liquid filtrate thus obtained
3. 3
   تركيزwas concentrated under reduced pressure
4. 4
   workup.ADDITIONTo the resulting residue, a saturated sodium hydrogen carbonate aqueous solution (15 ml) was added
5. 5
   استخلاصtwo 50 ml methylene chloride extractions
6. 6
   تجفيفThe resulting organic layer was dried with anhydrous magnesium sulfate
7. 7
   ترشيحMagnesium sulfate was filtered off
8. 8
   تركيزthe liquid filtrate was concentrated under reduced pressure

الإجراء التجريبي

The N,N-dibenzyl-(1R,2S,4S)-1-methyl-2-hydroxy-4-phenylhexyl amine (1.46 g, 3.77 mmol) obtained above was dissolved in methanol (25 ml). Subsequently, acetic acid (0.43 ml, 7.53 mmol) and 5% Pd-C (palladium carbon; containing 50% of water) (0.6 g) were added to the dissolved solution. This reaction solution was stirred for 16 hours at 50° C. under a hydrogen atmosphere, and the catalyst was filtered off. The liquid filtrate thus obtained was concentrated under reduced pressure. To the resulting residue, a saturated sodium hydrogen carbonate aqueous solution (15 ml) was added and two 50 ml methylene chloride extractions were performed. The resulting organic layer was dried with anhydrous magnesium sulfate. Magnesium sulfate was filtered off and the liquid filtrate was concentrated under reduced pressure to yield (1R,2S,4S)-1-methyl-2-hydroxy-4-phenylhexyl amine (0.61 g, 2.96 mmol).

المصدر