Dicofol synthesis

Yield:-

Reaction Conditions:

Stage #1:p,p'-DDT in acetonitrile at 20;Inert atmosphere;UV-irradiation;
Stage #2: with oxygen in acetonitrilechemoselective reaction;

Steps:

2.2. Procedures
Reaction mixture was a suspension of DDT (5.73 mg = 1.6 × 10^{- 5} mol) in 10 mL acetonitrile, containing 10 mg of the Complex (1). Each experimental cycle was consisted of two consecutive periods: in the first period, the reaction mixture while stirring was exposed under UV-irradiation, in argon atmosphere and in the absence of dioxygen during 6-7 h, then, in the second period, the reaction was carried out without UV-irradiation and in the presence of dioxygen (“dark” period, 2-2.5 h). Before the beginning of a new experimental cycle, dioxygen was thoroughly removed from the reaction mixture during 1.5-2 h. All experiments were carried out at room temperature. Identification and analysis of the products were carried out by gas-liquid chromatography (electron capture detector), using column with SE-30 sorbent, the control analysis were carried out by chrommass-spectrometer DANI Master DC TOF, using capillary column (30 m) coated by DB-ALC2. Analysis of Cl-ions were performed by chemical methods (argentometric way by the Mohr method).

References:

Bakhtchadjian;Manucharova;Tavadyan [Catalysis Communications,2015,vol. 69,p. 193 - 195]

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