反应详情

To a 250 mL round bottomed flask which contained a suspension of Pd—C (10% wt 3 g) in EtOH (70 mL) and THF (30 mL) was added (R)-2-(4-benzyloxy-phenoxymethyl)-pyrrolidine-1-carboxylic acid tert-butyl ester (3.5 g, 9 mmol). The stirred solution was flushed with a H2 balloon. This process was repeated 3 times. The resulting solution was stirred at rt under hydrogen atmosphere overnight. The reaction mixture was then filtered, washed with THF (30 ml), EtOH (25 ml) and dried in vacuo to provide the crude product which was further purified by recrystallization with ether-EtOAc-hexane to yield the title product, (2.5, 90%); MS; APCI+, Calcd: 293.5. Found m/z: 294.2 (M+1). 1H NMR (400 MHz, CDCl3); δ 1.47 (s, 9H), 1.80-2.10 (m, 4H), 3.40 (br, 2H), 3.69-3.89 (m, 1H), 4.00-4.18 (m 2H), 6.71-6.76 (m, 4H).

1. customTo a 250 mL round bottomed flask which contained
2. customThe stirred solution was flushed with a H2 balloon
3. filtrationThe reaction mixture was then filtered
4. washwashed with THF (30 ml), EtOH (25 ml)
5. customdried in vacuo
6. customto provide the crude product which
7. customwas further purified by recrystallization with ether-EtOAc-hexane