The structure of organophosphorus compounds. Part XLIV. The molecular structure of the 2-methylphenyl ester of N-[2, 4, 6-tri(tert-butyl) phenyl] imidophosphenous acid

Part XLIII, see ref. [1].     

The structure of organophosphorus compounds. Part XLIII. The molecular structure of cis- and trans-λ3-amino-2,4,6 -tri(Tert-Butyl)Phenyliminophosphines

Part XLII, see ref. [1].     

双(2,6-二叔丁基-4-甲基苯基)季戊四醇二磷酸酯的合成

以季戊四醇(1),三氯化磷(2)和2,6-二叔丁基对甲酚(3)为原料,三乙胺为催化剂和缚酸剂,经一锅法合成了双(2,6-二叔丁基-4-甲基苯基)季戊四醇二磷酸酯(PEP-36),其结构经1H NMR,13C NMR,IR和ESI-MS确证。采用正交试验对反应条件进行了优化。在最佳反应最佳条件[三乙胺为催化剂和缚酸剂,1 100 mmol,n(1)∶n(2)∶n(3)=1.0∶2.4∶2.4,于110℃反应12 h后于125℃反应12 h]下,PEP-36的收率70.2%,纯度99.07%。     

Synthesis and structure of 2,6-di-tert-butyl-1,4-benzoquinone-4N-(8-tosylamino-1-naphthyl) imine

The structure of 2,6-di-tert-butyl-1,4-benzoquinone-4-N-(8-tosylamino-1-naphthyl)imine (IId) has been studied as a model for the open form of thermoand photochromic compounds in the cyclohexadienoneperimidine series (I), in which rearrangement occurs due to C_spiro-N bond cleavage and N N proton transfer upon thermal or photoexcitation. Introduction of a bulky, electronwithdrawing tosyl substituent to the nitrogen atom stabilizes the open quinoneimine form, both in the crystalline state and in solution. The cyclohexadienone fragment is nonplanar and exists in a boat configuration. The open quinoneimine structure is retained upon replacement of the tosyl substituent by a less bulky electron-withdrawing acetyl substituent, suggesting that electronic factors are decisive in formation of the open structure.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 8, pp. 1802–1808, August, 1991.     

Synthesis and Crystal Structure of N-[4-(4-Methyl-phenylsulfamoyl)-phenyl]-4-methyl-1,2,3-thiadiazole-5-carboxamide

The crystal structure of the title compound (C17H16N4O3S2, Mr = 388.46) has been determined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 13.688(2), b = 16.704(3), c = 8.3308(12) , β = 99.474(6)o, V = 1878.8(5) 3, Mr = 388.46, Z = 4, Dc = 1.373 g/cm3, μ = 0.308 mm–1, F(000) = 808, R = 0.0389 and wR = 0.0917. X-ray analysis reveals that the crystal structure involves intermolecular N–H…O and N–H…N hydrogen bonds, which link the molecules into a layer parallel to the ac plane.     

3-[N-(4-甲基苯基)氨基羰基]-5-[4-(4-甲酸基苯甲氧基)苯亚甲基]-2,4-噻唑烷二酮的合成

以对甲苯胺和对甲基苯甲酸甲酯为起始原料,经NBS溴化、亲核取代、酸水解和Knoevenagel缩合等6步反应合成了抗细菌生物膜化合物—3-[N-(4-甲基苯基)氨基羰基]-5-[4-(4-甲酸基苯甲氧基)苯亚甲基]-2,4-噻唑烷二酮,总收率57.3％,其结构经1H NMR,ESI-MS和元素分析确证.     

Generation and Reactions of Lithiated tert-Butyl and 2,6-Di(tert-butyl)-4-methylphenyl Cyclopropanecarboxylates

tert-Butyl and 2,6-di(tert-butyl)-4-methylphenyl (BHT) cyclopropanecarboxylates ( 4 , 6 , 24 , 25 ) are lithiated with LiN(i-Pr)₂ and t-BuLi, respectively. Reactions with alkyl halides, aldehydes, acyl chlorides, and heteroelectrophiles give α-substituted BHT esters which can be cleaved (t-BuOK/H₂O/THF) to the corresponding carboxylic acids or reduced (LiAlH₄/THF) to the cyclopropanemethanols.