反应详情

温度

-78 °C

A solution of N-benzyl-(+)-methyl-benzylamine (8.5 mL, 40.4 mmol) in THF (100 mL) was cooled to 0° C., then n-butyl lithium (16 mL, [2.5 M], 40.4 mmol) was added and the resulting mixture stirred for 1 hour. The reaction mixture was cooled to −78° C., then a solution of 3-cyclohexyl-acrylic acid tert-butyl ester (7.71 g, 36.7 mmol) in THF (20 mL) was added dropwise for 30 min and the resulting mixture was stirred an additional 1 hour at −78° C. The reaction was quenched with NH4CT (s), and extracted with EtOAc, the organic layer was dried with MgSO4, filtered and evaporated under reduced pressure to yield a residue. The residue was purified by column chromatography (10%-70% EtOAc/heptane) to yield a residue.

1. stirringthe resulting mixture was stirred an additional 1 hour at −78° C
2. customThe reaction was quenched with NH4CT (s)
3. extractionextracted with EtOAc
4. dry with materialthe organic layer was dried with MgSO4
5. filtrationfiltered
6. customevaporated under reduced pressure
7. customto yield a residue
8. customThe residue was purified by column chromatography (10%-70% EtOAc/heptane)
9. customto yield a residue