E-2-CHLORO-8-METHYL-3-(2-NITRO)VINYLQUINOLINE synthesis

Yield:1031929-18-6 75.6%

Reaction Conditions:

with mesoporous nickel hydroxyapatite nanocomposite for 0.0166667 h;Microwave irradiation;Neat (no solvent);Henry reaction;

Steps:

General procedure: To an equimolar mixture of respective aldehydes and nitromethane (0.5 mM), 50 mg of Ni-HAp catalyst was added and irradiated in a closed vessel under 160 W microwave radiation for 1 min as given in Scheme 1. Then, the reaction mixture was extracted with methanol and quantified by GC-MS. The catalyst separated was washed several times with methanol, dried at room temperature, and subjected to reusability test. Gas chromatograph equipped with 5% diphenyl and 95% dimethyl siloxane, Elite 5MS (60 m length, 0.25 mm dia), and a mass detector (MS) with helium as a carrier gas was used for the quantification of products. The initial column temperature was increased from 80 to 160 °C at a rate of 10 °C/min and then to 280 °C at the rate of 40 °C/min. The temperatures of the injection port and transfer line were kept constant at 280 and 250 °C, respectively, during the product analysis.

References:

Neelakandeswari;Sangami;Emayavaramban;Karvembu;Dharmaraj;Kim, Hak Yong [Tetrahedron Letters,2012,vol. 53,# 24,p. 2980 - 2984] Location in patent:experimental part