反应详情

To a stirred solution of 3.05 g (0.0089 mol) of product of example 1 and 0.094 g (0.01 mol) of methyl chloroformate in 25 mL dry THF was added 1.16 g (0.012 mol) of triethylamine dropwise at room temperature. After stirring for 30 min, the solvent was evaporated under reduced pressure. The residue was diluted with 100 mL of water and extracted with ether (3×50 mL). The combined organic layers were washed with water, dried (MgSO4) and evaporated. Purification of the residue by preparative HPLC (5% ethyl acetate-hexane) gave 2.75 g (77%) of product as a yellow oil: nD25 1.5830.

1. customthe solvent was evaporated under reduced pressure
2. additionThe residue was diluted with 100 mL of water
3. extractionextracted with ether (3×50 mL)
4. washThe combined organic layers were washed with water
5. dry with materialdried (MgSO4)
6. customevaporated
7. customPurification of the residue by preparative HPLC (5% ethyl acetate-hexane)