反应详情

温度

0 °C

To a solution of ethyl 9-bromo-2,2-dimethylnonanoate (example 103, step a) (1.27 g) in dry diethyl ether (40 mL) at 0° C. under N2 was added diisobutylaluminium hydride (1 M in toluene, 9.5 mL) dropwise. The reaction mixture was stirred at 0° C. for 1.25 h then quenched by addition of saturated potassium sodium tartrate solution (150 mL). The mixture was stirred for 15 min then extracted with ethyl acetate (×3) then the combined organics were washed with brine, dried over sodium sulphate, filtered and evaporated in vacuo. Purification was by silica gel chromatography eluting with 0-25% ethyl acetate in cyclohexane to give the subtitled compound as a colourless liquid. Yield 0.56 g.

1. customthen quenched by addition of saturated potassium sodium tartrate solution (150 mL)
2. stirringThe mixture was stirred for 15 min
3. extractionthen extracted with ethyl acetate (×3)
4. washthe combined organics were washed with brine
5. dry with materialdried over sodium sulphate
6. filtrationfiltered
7. customevaporated in vacuo
8. customPurification
9. washeluting with 0-25% ethyl acetate in cyclohexane