反应详情

温度

-78 °C

To a solution of ester from Step 2 (16.0 g, 39.8 mmol) in CH2Cl2 (320 mL) at -100° C. was added slowly a solution of DIBAH (1.5M/toluene, 32 mL, 47.7 mmol). The reaction was then stirred for 1-- h at -78° C., before being quenched by the addition of MeOH (3 mL), followed by 25% w/v tartaric acid (100 mL). After stirring overnight at r.t., the product was extracted with CH2Cl2. The organic layer was dried (MgSO4), filtered, and evaporated to give a pale green syrup. This was stirred vigorously with 1:4 Et2O/hexane to give 13 g of the title compound as an off-white solid.

1. custombefore being quenched by the addition of MeOH (3 mL)
2. stirringAfter stirring overnight at r.t.
3. extractionthe product was extracted with CH2Cl2
4. dry with materialThe organic layer was dried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customto give a pale green syrup