9002-98-6Relevant articles and documents
Method for synthesizing fluopyram
-
Paragraph 0018; 0033-0036; 0040-0041, (2021/09/26)
The invention provides a method for synthesizing fluopyram, which uses commercially available 2 - bromoethylamine hydrobromide as a starting raw material, generates cyclopropylamine by self nucleophilic substitution reaction under basic conditions, and then reacts with o-trifluorobenzoyl chloride to prepare the key intermediate cyclopropylamine -1 -(2 - (trifluoromethyl) phenyl) methyl ketone. 2,3 -dichloro -5 -trifluoromethylpyridine was reacted with cyclopropylamine -1 -based (2 - (trifluoromethyl) phenyl) methyl ketone after the action of alkyllithium to give fluopyram. 1st-step and 2nd-step reactions are one-pot reaction, the reaction yield is high, the synthesis process is simple, the product purity is high, and the method has huge application value.
Barium complexes with crown-ether-functionalised amidinate and iminoanilide ligands for the hydrophosphination of vinylarenes
Le Coz, Erwann,Roueindeji, Hanieh,Roisnel, Thierry,Dorcet, Vincent,Carpentier, Jean-Francois,Sarazin, Yann
supporting information, p. 9173 - 9180 (2019/07/04)
The detailed multistep syntheses of two nitrogen-based sterically congested iminoanilidine and amidine proligands bearing a tethered 15-member aza-ether-crown macrocycle, namely {I^Acrown}H and {Amcrown}H, are reported. These proligands react with [Ba{N(SiMe2H)2}2·(thf)n] to generate the heteroleptic barium complexes [{I^Acrown}BaN(SiMe2H)2] (5) and [{Amcrown}BaN(SiMe2H)2] (6) in high yields. These complexes exhibit high coordination numbers (resp. eight and seven) and are in addition stabilised by mild Ba?H-Si interactions. Unusually for oxophilic elements such as barium, the amidinate ligand in 6 is only η1-coordinated. Complexes 5 and 6 mediate the intermolecular hydrophosphination of styrene with primary (PhPH2) and secondary (HPPh2) phosphines. Their catalytic performance compares favourably with those of other barium precatalysts for these reactions. During the course of the hydrophosphination of styrene with HPPh2 catalysed by 5, the phosphide complex [{I^Acrown}BaPPh2] (7) could be intercepted and crystallographically characterised.
Method for preparing thiotepa
-
Paragraph 0049; 0050, (2018/09/21)
The invention provides a method for preparing thiotepa. The method comprises the following steps: cooling ethylenimine and an organic solvent to a temperature of 15-17 DEG C, dropping an organic solvent of trihalothiophosphorus, dropping an acid-binding agent when the trihalothiophosphorus is dropped to reach a scheduled quantity Y of 49%, maintaining the temperature of 15-17 DEG C, and reacting for 30-45 minutes; filtering, performing reduced pressure distillation on the filtrate to remove the organic solvent so as to obtain the residue, and purifying, so as to obtain the thiotepa. The raw materials and reagent used in the preparation method provided by the invention are cheap and readily available, the produced three wastes are less, and the method is simple in operation, high in yield and suitable for industrial production.
