反应详情

A solution of methyl 1-[4-(4-chlorophenyl)piperazine-1-sulfonyl]piperidine-2-(RS)-carboxylate (164 mg, 0.41 mmol), [prepared as described in Example 3] and NaOH (33 mg, 0.82 mmol) in methanol/water (5 ml of 9:1 ratio) was heated at reflux. After 2 h, the reaction mixture was concentrated in vacuo, diluted with water (5 ml) and extracted with diethyl ether. The aqueous phase was acidified to pH 3 with 5% potassium bisulfate solution and the product was extracted into ethyl acetate. The organic phase was washed with brine, dried over MgSO4, and concentrated to yield 1-[4-(4-chlorophenyl)piperazine-1-sulfonyl]piperidine-2-(RS)-carboxylic acid as a foam (125 mg, 79%).

1. temperaturewas heated
2. temperatureat reflux
3. concentrationthe reaction mixture was concentrated in vacuo
4. additiondiluted with water (5 ml)
5. extractionextracted with diethyl ether
6. extractionthe product was extracted into ethyl acetate
7. washThe organic phase was washed with brine
8. dry with materialdried over MgSO4
9. concentrationconcentrated