A new method for synthesizing 2,6-dichlorodiphenylamine was presented in this article.2,6-dichlorodiphenylamine is the key intermediate for the preparing of diclofenac sodium.It was synthesized in a one-shot reaction ...A new method for synthesizing 2,6-dichlorodiphenylamine was presented in this article.2,6-dichlorodiphenylamine is the key intermediate for the preparing of diclofenac sodium.It was synthesized in a one-shot reaction with 2,6-dichlorophenol,a solution of sodium methoxide in methanol,methyl chloroacetate,aniline,and sodium hydroxide as raw materials by the acid-base neutralization,etherification,ammonolysis of ester,Smiles rearrangement of amide,and alcoholysis or hydrolysis of the rearrangement product.Based on many times of experiment,the best technological condition was found.The yield of target compound was about 91%.展开更多
A dinuclear manganese(Ⅱ) complex, [Mn2(L1)2(phen)4]·(ClO4)2 (1), has been synthesized and structurally characterized (HL1=2,6-dichlorobenzoic acid, phen=1,10-phenanthroline). It crystallizes in triclinic system,...A dinuclear manganese(Ⅱ) complex, [Mn2(L1)2(phen)4]·(ClO4)2 (1), has been synthesized and structurally characterized (HL1=2,6-dichlorobenzoic acid, phen=1,10-phenanthroline). It crystallizes in triclinic system, space group P1 with a=1.112 3(4) nm, b=1.378 2(4) nm, c=2.085 7(3) nm, α=93.768(2)°, β=90.606(10)°, γ=95.606(3)°, V=3.174 8(15) nm3, Z=2, C62H38Cl6Mn2N8O12, Mr=1 409.58, Dc=1.475 g·cm-3, μ=0.718 mm-1, F(000)=1 428, R=0.064 3, wR=0.138 3. In the crystal the manganese atom is six-coordinated by two oxygen atoms from two different 2,6-dichlorobenzolate molecules and four nitrogen atoms from two 1,10-phenanthroline molecules, completing an octahedral geometry. CCDC: 692296.展开更多
文摘A new method for synthesizing 2,6-dichlorodiphenylamine was presented in this article.2,6-dichlorodiphenylamine is the key intermediate for the preparing of diclofenac sodium.It was synthesized in a one-shot reaction with 2,6-dichlorophenol,a solution of sodium methoxide in methanol,methyl chloroacetate,aniline,and sodium hydroxide as raw materials by the acid-base neutralization,etherification,ammonolysis of ester,Smiles rearrangement of amide,and alcoholysis or hydrolysis of the rearrangement product.Based on many times of experiment,the best technological condition was found.The yield of target compound was about 91%.
文摘A dinuclear manganese(Ⅱ) complex, [Mn2(L1)2(phen)4]·(ClO4)2 (1), has been synthesized and structurally characterized (HL1=2,6-dichlorobenzoic acid, phen=1,10-phenanthroline). It crystallizes in triclinic system, space group P1 with a=1.112 3(4) nm, b=1.378 2(4) nm, c=2.085 7(3) nm, α=93.768(2)°, β=90.606(10)°, γ=95.606(3)°, V=3.174 8(15) nm3, Z=2, C62H38Cl6Mn2N8O12, Mr=1 409.58, Dc=1.475 g·cm-3, μ=0.718 mm-1, F(000)=1 428, R=0.064 3, wR=0.138 3. In the crystal the manganese atom is six-coordinated by two oxygen atoms from two different 2,6-dichlorobenzolate molecules and four nitrogen atoms from two 1,10-phenanthroline molecules, completing an octahedral geometry. CCDC: 692296.
