|
With dmap; triethylamine; In 1,2-dichloro-ethane; at -5 - 5℃; for 2.5h; |
Step 2:2L four bottles of the first step to add 200.8g (1179.0mmol, 1.0eq), 800.0 g of dichloroethane, 131.2 g (1279.0 mmol, 1.1 eq) of triethylamine, 14.4 g (117.8 mmol, 0.1 eq) of 4-dimethylaminopyridine,Into the ice machine cooling to -5 ~ 0 stand.A solution of 148.6 g (1297.0 mmol, 1.1 eq) of methanesulfonyl chloride and 200.8 g of dichloroethane was added dropwise over 1.5 h, and the dropping temperature was controlled at -5 to 5 C,Followed by 0 ~ 5 insulation stirring 1.0h.Add water 600g quenching reaction, then stop the cooling, the kettle temperature to room temperature, stirring 0.5h, standing for 0.5h, divided into an oil layer 1268.0g, the water back to the kettle by adding dichloroethane 200.0g secondary extraction, stirring 0.5 h, standing for 0.5h, separate the secondary reservoir 188.7g.Combined with a secondary oil layer, add water 400.0g washing, stirring 0.5h, standing for 0.5h, separated from the oil layer, desolvation, the use of ethanol to get 260.0g two-step product, the content of> 98%, yield 88% Cis - trans isomer ratio 56/44. |