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ChemicalBook CAS DataBase List Toremifene
89778-26-7

Toremifene synthesis

4synthesis methods
97151-03-6 Synthesis
1,2-Diphenyl-1-[4-[2-(Dimethylamino) Ethoxy]-Phenyl] Butane-4-Ol

97151-03-6
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Yield:89778-26-7 106 g

Reaction Conditions:

with thionyl chloride in toluene at 0 - 110; for 3 h;Temperature;

Steps:

3
To a 5L reaction flask 2. 2L of toluene, 110g (0. 28mol) obtained in the above step Z configuration compound F,mixed to obtain a sixth system, the temperature was lowered to 0~5 ° C Mixture VI , was slowly added dropwise 66. 62g (0.56mol) thionyl chloride addition was complete the formation of the seventh mixed system, the mixed system was slowlywarmed to a seventh 110° C, 3 hours the reaction product obtained after the third system, stop The third product heatingand cooling system to 15~25 ° C, the third product system slowly poured into 1L of water, adding NaOH solution to a pH9~10 and get the second system, the second in and a system for liquid separation, and the resulting aqueous phase wasextracted 2L MTBE to give a second extract was concentrated organic phases were combined and dispensing a secondextraction solution to give the toremifene crude, the crude by the mass ratio of 1: 1 mixture of acetone and methanol solventcrystallization to give 106g toremifene product.

References:

ASYMCHEM LAB FUXIN INC;ASYCHEM PHARMACEUTICALS TIANJIN CO LTD;Hong, Hao;Gaigi, James;Li, jiuyuan;Zhang, Enxuan CN104230723, 2016, B Location in patent:Paragraph 0063; 0068; 0069

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