反应详情

To a solution of 1-tert-butoxycarbonyl-2(S)-(2-hydroxyethyl)piperazine (0.479 g, 2.08 mmol) in DMF was added EDC.HCl (0.432 g, 2.25 mmol), HOBT (0.314 g, 2.05 mmol) and naphthalene-2-carboxylic acid (0.353 g, 2.05 mmol). Triethylamine was added to pH 7. The reaction was stirred overnight at room temperature. The DMF was removed in vacuo and the residue dissolved in 1:1 methanol-tetrahydrofuran and 5% sodium hydroxide added. The reaction was stirred several hours, the solvent evaporated and the residue partitioned between ethyl acetate and 5% sodium hydroxide. The organic phase was dried over magnesium sulfate and the crude product thus obtained chromatoraphed on silica gel with 50% ethyl acetate in hexane. The title compound was obtained as a white foam.

1. customThe DMF was removed in vacuo
2. dissolutionthe residue dissolved in 1:1 methanol-tetrahydrofuran and 5% sodium hydroxide
3. additionadded
4. stirringThe reaction was stirred several hours
5. customthe solvent evaporated
6. customthe residue partitioned between ethyl acetate and 5% sodium hydroxide
7. dry with materialThe organic phase was dried over magnesium sulfate
8. customthe crude product thus obtained