The reaction of bromo- and iodo-phosphoranes with unactivated coarse grain manganese metal powder to yield [MnI2(phosphine)2] and [{MnX2(phosphine)}n](X = Br or I) by insertion of Mn into the P–X bond. The crystal structure of [MnI2(PPh3)2]
摘要:
The novel reaction of crude manganese metal powder with dibromo- and diiodo-phosphoranes, R3PX2, has been studied. Reaction of the phosphoranes R3PI2 (R = phenyl or substituted aryl) with manganese allows insertion of the metal into P-X bonds and gives the monomeric tetrahedral complexes [MnI2(PR3)2] and MnI2. However, reaction of R3PX2 (R3 = mixed aryl/alkyl, trialkyl; X = Br or I) with manganese, whilst once again proceeding via insertion into P-X bonds, now leads to the quantitative isolation of the polymeric complexes [{MnX2(PR3)}n], thus illustrating the subtle nature of these reactions. Examples of both types of complex have been crystallographically characterised and represent rare examples of such. There is some evidence that where R3 = Ph2Me an equilibrium exists and both types of complex, [MnI2(PPh2Me)2] and [{MnI2(PPh2Me)}n] can be detected from the same reaction.
Multiple metal-carbon bonds. 8. Preparation, characterization, and mechanism of formation of the tantalum and niobium neopentylidene complexes, M(CH2CMe3)3(CHCMe3)
[EN] AN IMPROVED PROCESS FOR THE PREPARATION OF DARIFENACIN HYDROBROMIDE<br/>[FR] PROCÉDÉ PERFECTIONNÉ POUR LA PRÉPARATION DE BROMHYDRATE DE DARIFÉNACINE
申请人:AUROBINDO PHARMA LTD
公开号:WO2011070419A1
公开(公告)日:2011-06-16
The present invention relates to an improved process for the preparation of Darifenacin hydrobromide of Formula (I). (i) condensing 3-(S)-(-)-1l-carbamoyl-1,1-diphenylmethyl)pyrrolidine (III), or its salt, with a compound of Formula XIII in the presence of a. base in a solvent, wherein X represents Cl, Br, C1-3 alkyl sulfonate or C6-10 arγl sulfonate; to produce (S)-2-[1-[2-(2,3-dihydrobenzofuran-5-yl)ethyl]-3- pyrrolidinyl]-2,2-diphenylacetamide (Darifenacin) (Ia), (ix) treating (S)-2-[1-[2-(2,3-dihydrobenzofuran-5-yl)ethyl]-3-pyrrolidinyl]- 2,2-diphenylacetamide (Darifenacin) (Ia) with an acid in a solvent and water mixture, (x) isolating pure (S)-2-[1-[2-(2,3-dihydrobenzofuran-5-yl)ethyl]-3- pyrrolidinyl]-2,2-diphenylacetamide (Darifenacin) (Ia), (xi) treating pure Darifenacin (Ia) with HBr to produce Darifenacin hydrobromide (I).
Methods and materials for preparing irreversible inhibitors of tyrosine kinases of general Formula 1 are disclosed. Such inhibitors, which include N-[4-(3-chloro-4-floro-phenylamino)-7-(3-morpholin-4-yl-propoxy)-quinazolin-6-yl]-acrylamide, are useful for treating cancer, restenosis, atherosclerosis, endometriosis and psoriasis. The disclosed methods employ protecting schemes to minimize undesirable diacryloylamino-quinazoline side products.
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