반응 #470343

반응 방정식

4-azidomethyl-2-(2-methylphenyl)benzoic acid methyl ester

→

desired product

수율 30.1%

4-Aminomethyl-2-(2-methylphenyl)benzoic acid methyl ester

수율 30.1%

용매

MeOH

반응 조건

후처리

1. 1
   workup.ADDITIONTo a flask at ambient temperature under N2 containing 10% palladium on carbon catalyst (1.0 g) was added
2. 2
   기타reaction
3. 3
   여과Catalyst filtered off through celite
4. 4
   세척washed with MeOH
5. 5
   농축Filtrate concentrated in vacuo, and residue
6. 6
   추출Aqueous solution extracted with CHCl3 (3×), and extracts
7. 7
   건조dried with Na2SO4
8. 8
   여과filtered
9. 9
   농축concentrated in vacuo

실험 절차

To a flask at ambient temperature under N2 containing 10% palladium on carbon catalyst (1.0 g) was added a solution of 4-azidomethyl-2-(2-methylphenyl)benzoic acid methyl ester (5.00 g, 17.8 mmol), prepared as in Example 1191A, in MeOH (75 mL). Two drops of conc. HCl added, and reaction stirred vigorously overnight under an atmosphere of H2. Catalyst filtered off through celite and washed with MeOH. Filtrate concentrated in vacuo, and residue taken up in an aqueous 4N NaOH solution. Aqueous solution extracted with CHCl3 (3×), and extracts dried with Na2SO4, filtered, and concentrated in vacuo to afford the desired product (1.37 g, 30%). m/e (DCI) 256 (MH+)

출처