Synthesis of an octamethyl-18-crown-6 derivative and the X-ray crystal structure of its 2:1 complex with borane-ammonia
作者:David R. Alston、J.Fraser Stoddart、John B. Wolstenholme、Billy L. Allwood、David J. Williams
DOI:10.1016/s0040-4020(01)96617-7
日期:1985.1
12,12-octamethyl-1,4,7,10,13,16-hexaoxacyclooctadecane (2) from pinacol (3) by a sequence of reactions (3→4→5→6+5→2) involving alkylation (3→ 4), ozonolysis and reduction (4→5), tosylation (5→6), and cyclisation (5+6→2) is reported. With borane-ammonia, the octamethyl-18-crown-6 derivative 2 forms a crystalline 2:1 complex, (BH3NH3)2 · 2. X-Ray crystallography reveals the two guest BH3NH3 molecules
通过一系列反应(3 → )从频哪醇(3)合成2,2,3,3,11,11,12,12-八甲基-1,4,7,10,13,16-六氧杂环丁烷(2)据报道,涉及烷基化(3 → 4),臭氧分解和还原(4 → 5),甲苯磺酸化(5 → 6)和环化(5 + 6 → 2)的4 → 5 → 6 + 5 → 2)。与硼烷-氨一起,八甲基-18-皇冠-6衍生物2形成结晶的2:1络合物,(BH 3NH 3)2 ·2。X射线晶体学分析显示,两个客体BH 3 NH 3分子以中心对称的方式与主体2的相对面氢键结合,并采用全乳胶(ag + ag - a)。3构象。