| 摘要 |
1,185,124. Alkylated halo-tin compounds; alkyl zinc halides. RHONE-POULENC S.A. 30 May, 1968 [31 May, 1967], No. 25952/68. Heading C2J. [Also in Division C3] Halo-tin compounds are alkylated by reacting with an alkyl zinc compound in an amide of the formula O=P(NRR) 3 or R<SP>1</SP>CONRR, where R and R<SP>1</SP> are C 1-4 alkyl radicals and R<SP>1</SP> may also be hydrogen. At least one mole of amide per atom of zinc should be present. Suitable tin compounds are those of the formula R a <SP>2</SP>-Sn-X 4-a where R<SP>2</SP> is a hydrocarbon radical which may be saturated or unsaturated, aliphatic or aromatic, or is an alkoxy radical, X is halogen and a is 0 to 3. Specified are SnCl 4 , CH 3 SnCl 3 , (CH 3 SnCl 2 , (C 2 H 5 )SnCl, (C 4 H 9 ) 2 SnCl 2 , (C 8 H 17 ) 2 SnCl 2 and Ph 2 SnCl 2 . The zinc compound may be a zinc dialkyl or alkyl zinc halide. The preferred amides are hexamethylphosphoryl triamide and N,N-dimethyl formamide. Reaction temperatures are generally from 10‹ to 120‹ C. and alkylation may be partial or complete. Examples 10 and 12 are relevant. Alkyl zinc halides are prepared by adding an alkyl halide to zinc in a hexa-alkylphosphoryl triamide, preferably in the presence of iodine or an alkyl iodide. This reaction may be carried out in situ with the alkylation of the tin compound. |
