CAS: 221011-41-2; 9,11,20,22-Tetrahydrotetrabenzo[d,F,K,M][1,3,8,10]Tetraazacyclotetradecine-10,21-Dithione

📜2,2-联苯二胺置于potassium Carbonate体系中,用 氯仿,水,N,N-二甲基甲酰胺 用作溶剂,化学反应 24.5H,反应生成9,11,20,22-四氢四苯并[d,F,K,M][1,3,8,10]四氮杂十四环-10,21-二硫酮
参考文献:Preparation And Intramolecular Cyclization Of Bis(Carbodiimides). Synthesis And X-Ray Structure Of 1,3-Diazetidine-2,4-Diimine Derivatives
标题:Preparation And Intramolecular Cyclization Of Bis(Carbodiimides). Synthesis And X-Ray Structure Of 1,3-Diazetidine-2,4-Diimine Derivatives
摘要:Aza-Wittig Reactions Of Bis(Iminophosphorane) 1 Derived From 2,2'-Diazidobiphenyl With Aromatic Isocyanates Provided Dibenzo[d,F]-1,3-Diazetidino[1,2-A]Diazepine Derivatives 2 In Moderate Yields. Similar Results Can Be Achieved From The Reaction Of 2,2'-Bis(Isothiocyanato)Biphenyl 4 With Aryliminophosphoranes. Treatment Of Bis(Isothiocyanate) 4 With Arylamines And Further Dehydrosulfurization Of The Resulting Bis(Thioureas) Leads To The Seven-Membered Ring Guanidines 8. N-2-(2'-Azido)Biphenyi-N'-Arylcarbodiimides 13 React With 1 Equiv Of Triphenylphosphane To Give Zwitterionic Compounds 15,Which Undergo Either Hydrolytic Cleavage To Afford The Guanidines 8 Or React With 1 Equiv Of Aromatic Isocyanates To Provide 2. Cross-Experiments Suggest That The: Conversion 15--> 2 Takes Place Through A Nonisolable Bis(Carbodiimide) That Undergoes An Intramolecular [2 + 2] Cycloaddition At The Final Step. The Reaction Of Bis(Iminophosphorane) 1 With An Excess Of Carbon Dioxide Leads To A Mixture Of The Tricyclic 1,3-Diazetidine Derivative 6 And The 14-Membered Cyclic Bis(Carbodiimide) 23,Which Decomposes By Thermal Treatment. Compound 6 Can Also Be Obtained Along With The Seven-Membered Cyclic Urea Derivatives 24 From The Reaction Of Bis(Iminophosphorane) 1 With The Carbon Dioxide Source Boc(2)O/dmap System. A Comprehensive Mechanistic Scheme For The Aza-Wittig Reactions Studied Is Conveniently Presented. The Molecular And Crystal Structures Of 1-(4-Methoxyphenyl)-2-(4-Methoxyphenyl)Iminodibenzo[d,F]-1,3-Diazetidino-[1,2-A]Diazepine (2C) And [a,C]Bis[dibenzo[d,F][1,3]Diazepino]-1,3]Diazepino]-1,3-Diazetidine (6) Have Been Determined By X-Ray Analysis.
Doi:10.1021/jo981339V