반응 #10289

반응 방정식

ammonium formate

(4S,5S)-5-(4-tert-butylphenyl)-4-methyl-oxazolidin-2-one

→

title compound

(S)-2-(4-tert-Butylphenyl)-1-methylethylamine

용매

methanol

반응 조건

후처리

1. 1
   온도was heated
2. 2
   온도under reflux for 2 hrs
3. 3
   여과The mixture was filtered
4. 4
   농축the filtrate was concentrated under reduced pressure
5. 5
   기타The residue was partitioned between 10 mL 10% sodium carbonate and 25 mL ethyl acetate
6. 6
   건조The organic phase was dried (magnesium sulfate)
7. 7
   농축concentrated under reduced pressure

실험 절차

A mixture of 1 g (4.3 mmole)(4S,5S)-5-(4-tert-butylphenyl)-4-methyl-oxazolidin-2-one p(see preparation 4, step 2), 2 g (31.74 mmole) ammonium formate and 0.1 g 10% palladium on carbon in 25 mL methanol was heated under reflux for 2 hrs. The mixture was filtered and the filtrate was concentrated under reduced pressure. The residue was partitioned between 10 mL 10% sodium carbonate and 25 mL ethyl acetate. The organic phase was dried (magnesium sulfate) and concentrated under reduced pressure. The title compound was isolated as the hydrochloride salt from diethyl ether, 0.93 g (95%), m.p.259.5–261.3° C.

출처