反应详情

The above prepared (2-acetyl-4-chloro-5-methoxy-phenoxy)-acetic acid ethyl ester-(6.05 g, 21.1 mmol) was dissolved in 45 mL of dimethoxyethane and treated at −15° C. with KOtBu (0.947 g, 0.4 eq.). After keeping for 45 Min. at −15° C. and 5 h at 0° C., the reaction mixture was poured onto crashed ice/HCl, twofold extracted with AcOEt, washed with water, dried over magnesium sulfate, and evaporated to dryness to leave 5.26 g of crude product. Flash chromatography (SiO2, hexane/AcOEt=9/1) of the latter afforded 2.32 g of the title compound as white crystals.

1. additionat −15° C. and 5 h at 0° C., the reaction mixture was poured
2. extractiontwofold extracted with AcOEt
3. washwashed with water
4. dry with materialdried over magnesium sulfate
5. customevaporated to dryness
6. customto leave 5.26 g of crude product