反应详情

温度

-30 °C

At −78° C., 104 ml of a 1.6M solution of butyl lithium were slowly added dropwise to 25 g (0.14 mol) of 4,4-dimethyl-2-phenyl-2-oxazolin and 0.1 g of triphenylmethane in 400 ml of anhydrous tetrahydrofuran. The mixture was stirred for 1 h. The mixture was then allowed to warm to −30° C. and a solution of 20.3 g (0.13 mol) of 2-naphthaldehyde in 200 ml of anhydrous tetrahydrofuran was added dropwise. Stirring was continued for about 1 h at −20 to −30° C. The reaction solution was then allowed to warm to room temperature and the solvent was removed under reduced pressure. The residue was introduced into ice-water which was then extracted with ether. The organic phase was dried and concentrated under reduced pressure. This residue was purified chromatographically (eluent: n-heptane/acetone=40/3), affording 25.3 g (54%) of the product.

1. stirringStirring
2. waitwas continued for about 1 h at −20 to −30° C
3. temperatureto warm to room temperature
4. customthe solvent was removed under reduced pressure
5. additionThe residue was introduced into ice-water which
6. extractionwas then extracted with ether
7. customThe organic phase was dried
8. concentrationconcentrated under reduced pressure
9. customThis residue was purified chromatographically (eluent: n-heptane/acetone=40/3)