反应详情

温度

-40 °C

Under an inert atmosphere a 50 mL four necked flask (flame dried) with a magnetic stirrer was charged with 990 mg (2.65 mmol) (3SR,4RS)-1-benzyl-3-(4-chloro-phenyl)-piperidine-4-carboxylic acid methoxy-methyl-amide in 15 ml THF. The light yellow solution was cooled to −40° C. and 2.2 mL methylmagnesium bromide (3M in diethyl ether) was added drop wise over 5 min. The reaction was slowly warmed up to 0° C. over 2 h. The reaction mixture was quenched slowly with 20 mL aqueous NH4Cl-solution, diluted with 10 mL water and 10 mL ethyl acetate. The aqueous layer was separated and extracted once with 30 mL ethyl acetate. The combined organic layers were washed with 50 mL brine, dried over Na2SO4, filtered off and concentrated under vacuum and used without further purification in the consecutive step. MS (m/e): 327.2 [(M+H)+].

1. temperatureThe reaction was slowly warmed up to 0° C. over 2 h
2. customThe reaction mixture was quenched slowly with 20 mL aqueous NH4Cl-solution
3. additiondiluted with 10 mL water and 10 mL ethyl acetate
4. customThe aqueous layer was separated
5. extractionextracted once with 30 mL ethyl acetate
6. washThe combined organic layers were washed with 50 mL brine
7. dry with materialdried over Na2SO4
8. filtrationfiltered off
9. concentrationconcentrated under vacuum
10. customused without further purification in the consecutive step