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温度

0 °C

A 250 ml round bottom flask equipped with magnetic stir bar and N2 inlet was charged with 7.8 g (27 mmole) 3-[(1-propylbutyl)sulfonyl]alanine and 7.4 g (30 mmole) N-Cbz succinamide in 100 ml methylene chloride. The reaction was cooled to 0° C., and 6.9 g NMM was added dropwise. The reaction was allowed to warm to room temperature and stirred for 4 hours at which point HPLC analysis indicated complete reaction. The reaction was concentrated in vacuo and partitioned between ethyl acetate and 1 N HCl. The organic layer was washed with water, brine, dried over sodium sulfate, and concentrated in vacuo to give 11.4 g of N-[(benzyloxy)carbonyl]-3-[(1-propylbutyl)sulfonyl]alanine that was used without further purification. M+H=386.

1. customA 250 ml round bottom flask equipped with magnetic stir bar and N2 inlet
2. temperatureto warm to room temperature
3. customreaction
4. concentrationThe reaction was concentrated in vacuo
5. custompartitioned between ethyl acetate and 1 N HCl
6. washThe organic layer was washed with water, brine
7. dry with materialdried over sodium sulfate
8. concentrationconcentrated in vacuo