HRID2226366
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
A mixture of 3.5 g of methyl (3R )-2-methyl-3-dodecanoyloxypentanoate, 12 ml of methanol and 0.5 ml of concentrated sulfuric acid was refluxed for 8 hours, and 20 ml of water was added thereto followed by ether extraction. The ether phase was dried over anhydrous sodium sulfate and ether was distilled away, and then the residue was distilled to give 0.6 g of methyl (3R)-2-methyl-3-hydroxypentanoate of the following formula, b.p. 52.5° C. (2.5 mm Hg), [α]D30 =-10.7° (C=0.61, CHCl3). ##STR97## This compound was converted to (+)-MTPA ester according to a procedure similar to Example 1-(5) and the optical purity determined by 1H-NMR was 95% ee. The NMR chart is shown in FIG. 4.
WORKUP
后处理
- temperaturewas refluxed for 8 hours
- extractionthereto followed by ether extraction
- dry with materialThe ether phase was dried over anhydrous sodium sulfate and ether
- distillationwas distilled away
- distillationthe residue was distilled