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General procedure: Various N,N-dimethyl benzamides were obtained followinga simple procedure which involves charging the reactionmixture containing benzyl alcohols (1mmol), catalyst(20wt%) and DMF (5mL) into a two necked 50mL roundbottom flask (RBF) and stirred for 10min at RT and then70% aqueous TBHP (5mmol) was introduced dropwiseto the mixture under continuous stirring at RT. The RBFwas fitted with a water condenser and heated for 24h at100C. After 24h, the reaction mixture was cooled to RTand catalyst was then separated by filtration. The reactionmixture was diluted with 100mL of DW and extractedusing ethyl acetate (2 × 60mL). The combined organiclayer was dried using Na2SO4and concentrated underrotatory evaporator. The crude products were purified bychromatography using silica gel, hexane and ethyl acetate.Similarly a range of N,N-substituted benzamides werealso obtained by taking the stoichiometric amount of variousN-substituted formamides in 5mL of toluene keepingother parameters constant.
With 1,8-diazabicyclo[5.4.0]undec-7-ene; at 80℃; for 3h;
General procedure: 2-Chloro-4-(trifluoromethyl)-benzonitrile(1.00 mmol) was dissolved in appropriate alcohol, and DBU(2.00 mmol) was added. The mixture was stirred for 3 h at 80 C.The reaction was quenched with water and extracted with EtOActwice. The combined organic extracts were dried over MgSO4,filtered, and concentrated in vacuo. The residue was purified byflash column chromatography on silica gel using EtOAc/hexane(1:4) eluant condition.
1-(4-fluorobenzyl)-5-chloropyridin-2-one[ No CAS ]
Yield
Reaction Conditions
Operation in experiment
93%
With 4-Fluorobenzyl bromide; at 130℃; for 12h;Green chemistry;
<strong>[4214-79-3]2-hydroxy-5-chloropyridine</strong> (0.259 g, 2 mmol), 4-fluorobenzyl alcohol (2.4 mmol,1.2 equiv.) And 4-fluorobenzyl bromide (0.0498 ml, 20 molpercent)were added successively to a tubular reactorSealed in air, and thenheated to 130 ° C for 12 hunder solvent-free conditions.After the TLC monitoring reaction was complete, the product was purified by column chromatography and the yield was 93percent
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