4,4'-Dimethoxytrityl chloride

100-66-3

98-07-7

40615-36-9

a. In a 500 L reactor, 75 kg of trichloromethylbenzene (M = 195.48, n = 383.67 mol) and 103.72 kg of anisole (M = 108.14, n = 959.17 mol) were added, followed by the addition of 53.35 kg of the catalyst aluminum chloride (M = 133.34, n = 400.1 mol). The reaction temperature was controlled to be 30 °C and the reaction was continuously stirred for 10 h to obtain the mixed reaction solution I. b. Add 475 kg of 5% dilute hydrochloric acid to the mixed reaction solution I at 30°C and transfer to a 1000 L reactor for hydrolysis reaction for 3 hours. Subsequently, 200 kg of dichloromethane was added, stirred well and stratified. After separating the organic phase, the aqueous phase was extracted twice with 200kg of dichloromethane. All organic phases were combined and dried with anhydrous sodium sulfate for 2 hours. c. Concentrate the dichloromethane to recover the solvent. 70.74 kg of epichlorohydrin (M = 126.93, n = 557.32 mol) was added and the reaction was carried out under reflux for 6 hours. After completion of the reaction, 130 kg of petroleum ether was added dropwise and cooled to 30°C for crystallization. Crude 4,4'-dimethoxytrityl chloride (DMT-Cl) was obtained by solid-liquid separation, and the HPLC purity of the crude product was 98.91%. d. The crude DMT-Cl was recrystallized with 4.5 times mass of dichloromethane and 20 times mass of petroleum ether, and the wet product was obtained by solid-liquid separation. The wet product was dried to give a final product DMT-Cl 110.66 kg with a purity of 99.95% and a yield of 85.13%. The recovered mixed solvent was quantitatively analyzed by gas chromatography (GC) and recycled.