反应详情

2-cyano-2-(2-nitro-5-phenoxy-benzyl)-hex-5-enoic acid ethyl ester (2.84 g, 7.20 mmol) was dissolved in methanol (42 mL). In a separate flask, LiOH (1.5 g, 36.0 mmol) was dissolved in water (21 mL). The LiOH solution was added to the methanolic solution containing 2-cyano-2-(2-nitro-5-phenoxy-benzyl)-hex-5-enoic acid ethyl ester and the reaction was allowed to stir at room temperature for 2 hours. Next, 12N HCl (3 mL) was added to the reaction mixture followed by removal of the methanol under reduced pressure. The reaction mixture was poured into a separatory funnel, ethyl acetate was added and the organic layer was washed 2 times with 1N HCl and one time with saturated brine solution. The organic layer was separated, dried with sodium sulfate, filtered and the solvent was removed to yield a residue.

1. customfollowed by removal of the methanol under reduced pressure
2. additionThe reaction mixture was poured into a separatory funnel
3. additionethyl acetate was added
4. washthe organic layer was washed 2 times with 1N HCl and one time with saturated brine solution
5. customThe organic layer was separated
6. dry with materialdried with sodium sulfate
7. filtrationfiltered
8. customthe solvent was removed
9. customto yield a residue