Preparation method of catalyst intermediate
A compound and time-fixed technology, applied in the field of preparation of catalyst intermediates, can solve the problems of unsuitable for pilot scale-up, weak selectivity, poor selectivity, etc., and achieve the effects of low cost, simple process, control and stability of ee value
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Embodiment 1
[0031] The preparation of embodiment 1 compound (II)
[0032] Add 600ml of dichloromethane and 100g of compound (I) into a 2L four-neck flask, stir and cool down to -10°C, add 22.6g of methanesulfonic acid dropwise at one time, stir for 0.5 hours, control the temperature below 0°C and slowly add Tf 2 O in dichloromethane (Tf 2 O: 132.90g, dichloromethane: 300ml), the dropwise addition is completed, and the control is sampled after 1 hour of heat preservation reaction;
[0033] After the reaction is complete, add 200ml of drinking water, adjust the pH to 7-8 with 10% aqueous sodium hydroxide solution, raise the temperature to 15°C, let stand to separate layers, wash the organic layer once with 200ml of drinking water, and evaporate the organic layer to dryness under reduced pressure to obtain the crude product ;
[0034] Add 900ml of methyl tert-butyl ether to the crude product, heat up to 55°C, keep stirring for 0.5 hours, cool down to 25°C, filter, and dry in vacuo to obtai...
Embodiment 2
[0035] The preparation of embodiment 2 compound (II)
[0036] Add 600ml of dichloromethane and 100g of compound (I) into a 2L four-neck flask, stir and cool down to -10°C, add 45.27g of methanesulfonic acid dropwise at one time, stir for 0.5 hours, control the temperature below 0°C and slowly add Tf 2 O in dichloromethane (Tf 2 O: 132.90g, dichloromethane: 300ml), the dropwise addition is completed, and the control is sampled after 1 hour of heat preservation reaction;
[0037] After the reaction is complete, add 200ml of drinking water, adjust the pH to 7-8 with 10% aqueous sodium hydroxide solution, raise the temperature to 15°C, let stand to separate layers, wash the organic layer once with 200ml of drinking water, and evaporate the organic layer to dryness under reduced pressure to obtain the crude product ;
[0038]Add 900ml of methyl tert-butyl ether to the crude product, raise the temperature to 55°C, keep stirring for 0.5 hours, cool down to 25°C, filter, and dry in ...
Embodiment 3
[0039] The preparation of embodiment 3 compound (II)
[0040] Add 600ml of dichloromethane and 100g of compound (I) into a 2L four-neck flask, stir and cool down to -10°C, add 31.81g of trifluoromethanesulfonic acid dropwise at one time, stir for 0.5 hours, and slowly add dropwise while controlling the temperature not exceeding 0°C Tf 2 O in dichloromethane (Tf 2 O: 132.90g, dichloromethane: 300ml), the dropwise addition is completed, and the control is sampled after 1 hour of heat preservation reaction;
[0041] After the reaction is complete, add 200ml of drinking water, adjust the pH to 7-8 with 10% aqueous sodium hydroxide solution, raise the temperature to 15°C, let stand to separate layers, wash the organic layer once with 200ml of drinking water, and evaporate the organic layer to dryness under reduced pressure to obtain the crude product ;
[0042] Add 900ml of methyl tert-butyl ether to the crude product, heat up to 55°C, keep stirring for 0.5 hours, cool down to 2...
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