(+-)-2-Butanol → Sec.-butyl 3-methyl-1,2,4-oxadiazol-5-yl-acetate
반응식
P(Cl)(Cl)(Cl)=O.[CH3:6][C:7]1[N:11]=[C:10]([CH2:12][C:13]([OH:15])=[O:14])[O:9][N:8]=1.[CH:16](O)([CH2:18][CH3:19])[CH3:17]>>[CH3:6][C:7]1[N:11]=[C:10]([CH2:12][C:13]([O:15][CH:16]([CH2:18][CH3:19])[CH3:17])=[O:14])[O:9][N:8]=1참가 물질
4
반응 조건
- 온도
- 65 °C
실험 절차
Using the procedure of Example 17, 12 g of phosphorous oxychloride were slowly added to a mixture of 12 g of 3-methyl-1,2,4-oxadiazol-5-yl-acetic acid and 8.9 g of dry sec.-butanol and the rate of addition was adjusted to a reaction temperature of 65°±5° C. The resulting reaction mixture was stirred for 90 minutes at 65° C., and then treated as in Example 17. The product was distilled at 68° C. and 1.5 mm Hg to obtain 6.1 g (35% yield) of sec.-butyl 3-methyl-1,2,4-oxadiazol-5-yl-acetate. The purity of the final product was about 95% (according to TLC and PMR spectrum) and it had a refractive index nD25 =1.438.