反应详情

To a solution of N-[(phenylmethoxy)carbonyl]-L-tryptophan 1,1-dimethylethyl ester (36 g; 98 mmol) in EtOH (150 mL) Pd/C 10% (5 g) was added. A H2 atmosphere was set and hydrogenation was performed with the aid of a Venturi type stirrer. Reaction conversion was estimated by HPLC (Chromatographic method L/46). After 6 h at r.t. the suspension was filtered through paper, then through Millipore® HA 0.45 μm and the filtrate was concentrated under reduced pressure to give a crude oil. The crude was dissolved in CHCl3 (200 mL) and washed with 5% aq. Na2CO3 (200 mL) and brine (150 mL). The organic layer was dried over Na2SO4 and concentrated to give L-tryptophan-1,1-dimethylethyl ester (18.16 g), which was used in the following step without further purification.

1. customReaction conversion
2. filtrationAfter 6 h at r.t. the suspension was filtered through paper
3. concentrationthrough Millipore® HA 0.45 μm and the filtrate was concentrated under reduced pressure
4. customto give a crude oil
5. washwashed with 5% aq. Na2CO3 (200 mL) and brine (150 mL)
6. dry with materialThe organic layer was dried over Na2SO4
7. concentrationconcentrated