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ChemicalBook CAS DataBase List Carbaryl

Carbaryl synthesis

11synthesis methods
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Yield:63-25-2 82%

Reaction Conditions:

with tert.-butylhydroperoxide;4,7-dimethoxy-1,10-phenanthroline;iron(II) bromide in decane at 20; for 2 h;Inert atmosphere;

Steps:

General procedure for the synthesis

General procedure: In a reaction vessel, 2ml of formamide was added to the phenol substrate and the solutionwas stirring over a period of 1 minute. On stirred add 5 mmol% of Iron (II)Bromide, and 5 mmol% 4,7-Dimethoxy- 1,10 phenanthroline to the above reaction mixture,then slowly add 3 mmol of TBHP (Oxidant) at room temperature. Then, raise thetemperature up to 60 C and allow the stirring for 4 hours under an inert atmosphere inpresence of molecular sieves. After completion of reaction time, the solvent wasremoved under reduced pressure or directly proceeded for the conventional work upwith ethyl acetate, water mixture. The organic layer was separated and dried overanhydrous Na2SO4. Removal of the solvent under reduced pressure afforded the crudeproduct, which was purified by column chromatography on silica gel using hexane andethyl acetate (8:2) mixture to afford the required product (3). TLC’s have to be monitoredby both UV and iodine

References:

Vala, Manoj Kumar;Sudhakar, Chithaluri;Adurthi, Suryakumari;Vanam, Shekhar [Synthetic Communications,2022,vol. 52,# 2,p. 250 - 257]

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