반응 #1265353

반응 방정식

compound 4

{2-[2-(2-{2-[2-(2-Azido-ethoxy)-ethoxy]-ethoxy}-ethoxy)-ethoxy]-ethoxy}-acetic acid tert-butyl ester

acetic acid

→

compound 5

수율 96.0%

{2-[2-(2-{2-[2-(2-Amino-ethoxy)-ethoxy]-ethoxy}-ethoxy)-ethoxy]-ethoxy}-acetic acid tert-butyl ester

수율 96.0%

용매

ethanol

반응 조건

후처리

1. 1
   여과filtered
2. 2
   기타to remove Pd/C
3. 3
   농축The filtrate was concentrated in vacuo
4. 4
   세척eluted with CH2Cl2:MeOH 20:1 to 10:1 (v/v)

실험 절차

To a solution of compound 4 (1.0 g, 2.4 mmol) in ethanol (20 mL) was added 10% Pd/C (0.3 g) and acetic acid (0.3 mL). The resulting mixture was stirred under an atmosphere of hydrogen for 16 hours and then filtered to remove Pd/C. The filtrate was concentrated in vacuo and the residue was loaded onto a silica gel gravity column (100 g) and eluted with CH2Cl2:MeOH 20:1 to 10:1 (v/v) to afford compound 5 as a oil (0.90 g, 96%).

출처