Compounds and their preparation methods, pharmaceutical intermediates and their applications
A compound and bromide technology, which is applied in the field of compound and its preparation, and pharmaceutical intermediates, can solve the problems of easy metal, residue, and metal pollution in products, and achieve the effects of eliminating metal residue, high yield, and mild reaction conditions
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Embodiment 1
[0044] A compound 001, that is, the compound numbered 001, the specific structural formula is:
[0045] Its concrete synthetic steps are as follows:
[0046] 1) At room temperature, add methyl phenyl sulfide (38.0mg, 0.3mmol) and methyl bromoacetate (281.0mg, 1.8mmol) successively to a pre-dried vial with a capacity of 4mL, and simultaneously add 0.3mL of 2,2,2-trifluoroethanol, and then placed in a reactor at 100°C for 24 hours;
[0047]2) Cool the reaction mixture after the reaction to room temperature (usually 25° C.). After the cooling is completed, the reaction system in the vial is directly transferred to a 10 mL eggplant-shaped bottle without post-treatment operation, and the Heidolph rotary evaporator (speed: 90rpm, the temperature is 40°C, the vacuum degree is 0.1Mpa), and the residue is subjected to column chromatography using 200-mesh column chromatography silica gel. The developer is petroleum ether and ethyl acetate, and petroleum ether: acetic acid The volume...
Embodiment 2
[0053] A compound 002, namely the compound numbered 002, the specific structural formula is:
[0054] Its concrete synthetic steps are as follows:
[0055] 1) At room temperature, add 4-chlorothioanisole (48.6mg, 0.3mmol) and methyl bromoacetate (281.0mg, 1.8mmol) successively to a pre-dried vial with a capacity of 4mL, and simultaneously add 0.3mL of 2,2,2-trifluoroethanol, and then placed in a reactor at 100°C for 24 hours;
[0056] 2) Cool the reaction mixture after the reaction to room temperature (usually 25° C.). After the cooling is completed, the reaction system in the vial is directly transferred to a 10 mL eggplant-shaped bottle without post-treatment operation, and the Heidolph rotary evaporator (speed: 90rpm, the temperature is 40°C, the vacuum degree is 0.1Mpa), and the residue is subjected to column chromatography using 200-mesh column chromatography silica gel. The developer is petroleum ether and ethyl acetate, and petroleum ether: acetic acid The volume ra...
Embodiment 3
[0061] A compound 003, namely the compound numbered 003, the specific structural formula is:
[0062] Its concrete synthetic steps are as follows:
[0063] 1) At room temperature, add methyl phenyl sulfide (38.0mg, 0.3mmol) and bromoacetonitrile (218.1mg, 1.8mmol) sequentially into a 4mL pre-dried vial, and simultaneously add 0.3mL of 2, 2,2-trifluoroethanol, and then placed on a reactor at 100°C for 24 hours;
[0064] 2) Cool the reaction mixture after the reaction to room temperature (usually 25° C.). After the cooling is completed, the reaction system in the vial is directly transferred to a 10 mL eggplant-shaped bottle without post-treatment operation, and the Heidolph rotary evaporator (speed: 90rpm, the temperature is 40°C, the vacuum degree is 0.1Mpa), and the residue is subjected to column chromatography using 200-mesh column chromatography silica gel. The developer is petroleum ether and ethyl acetate, and petroleum ether: acetic acid The volume ratio of ethyl est...
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