1: diethoxyphosphoryl-acetic acid ethyl ester With sodium hydride in tetrahydrofuran
Cooling with ice;
2: pivalaldehyde in tetrahydrofuran
T=20°C; 48 h;
3: With ammonium chloride in tetrahydrofuran; water
参考文献
Institute Of Medicinal Molecular Design, Inc.; ShionogiandCo., Ltd.
Patent: EP2208728 A1, 2010 ;
Location in patent: Page/Page column 172 ;
tetrabutyl ammonium fluoride in tetrahydrofuran
soln. of TBAF is added to soln. of ethyl (trimethylgermyl)(trimethylsilyl)acetate and trimethylacetaldehyde in THF at -78°C (N2), stirring for 1 h; addn. of ether, washing (aq.NaCl), drying (MgSO4), concn., chromy. (silica gel, hexane/ether);
sodium tetrahydroborate
1.) benzene, irradiation; Yield given. Multistep reaction. Yields of byproduct given. Title compound not separated from byproducts;
参考文献
Russell, Glen A.; Shi, Bing Zhi; Jiang, Wan; Hu, Shuiesheng; Kim, Byeong H.; Baik, Woonphil
Journal of the American Chemical Society, 1995 , vol. 117, # 14 p. 3952 - 3962