规格:95%
外观:棕色固体
用途:基础原料、有机中间体、医药中间体
合成工艺如下:
1,4-dioxane;
Reactants are commercially availlable.
SCHERING CORPORATION, WO2008/54702, A1, (2008) EXAMPLE 32Preparation of Intermediate Compound 32AA mixture of 3-bromopyruvic acid (16.37 g, 98.05 mmol) in anhydrous dioxane (90 ml_) was treated with ethyl thioamidooxalate (13.08 g, 98.22 mmol) for 1.2 h at 50 0C, and was then concentrated at 50 0C to yield a dry yellow solid. The crude product was dissolved in saturated sodium bicarbonate (150 mL) and water (150 mL). This solution was extracte d with ethyl acetate (6 x 400 mL). The aqueous EPO layer was then acidified to pH 2 with concentrated aqueous HCI (21 ml_), resulting in the formation of a heavy precipitate. This suspen sion was extracted with ethyl acetate (5 x 500 ml_). These extracts were pooled, dried with sodium sulfate, filtered, concentrated, and dried for about 15 hours under vacuum to yield compound 32A as a red-brown solid (14.36 g, 73percent yield) which was used without further purification.
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