Synthetic method of oxazoline medical intermediate compound
A synthesis method and compound technology, which are applied in the fields of organic synthesis, synthesis of oxazoline compounds, and synthesis of heteroatom-containing compounds, can solve the problems such as the reaction yield needs to be improved, the scope of application is narrow, etc., and achieve wide application prospects and industrialization. The effect of applying potential
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0039]
[0040] At room temperature, add 100 mmol of the above formula (I) compound, 4 mmol of the catalyst 1-benzyl-3-methylimidazolium bromide, 100 mmol of p-nitrobenzenesulfonic acid, and 10 mmol of the above-mentioned organic phosphine ligand L1 to an appropriate amount of organic solvent DMSO and 100 mmol 2-iodoethyl methyl ether, and the temperature was raised to 40° C. and the reaction was stirred at this temperature for 8 hours.
[0041] After the reaction, the pH value of the reaction solution was adjusted to 7-7.5 with a 10% NaOH aqueous solution with a concentration of 10% by mass, then fully washed 2-3 times with deionized water, then extracted 2-3 times with dichloromethane, and combined organic phase, dried with anhydrous sodium sulfate, filtered, the filtrate was concentrated in vacuo, and the residue was subjected to 300-400 mesh silica gel column chromatography, using a mixture of ethyl acetate and chloroform with a volume ratio of 1:2 as the eluent, thereby...
Embodiment 2
[0044]
[0045]At room temperature, add 100mmol of the above formula (I) compound, 8mmol catalyst 1-benzyl-3-methylimidazolium chloride, 125mmol p-nitrobenzenesulfonic acid, 20mmol of the above-mentioned organic phosphine ligand L1 to an appropriate amount of organic solvent DMSO and 150 mmol 2-iodoethyl methyl ether, and the temperature was raised to 60° C. and the reaction was stirred at this temperature for 6 hours.
[0046] After the reaction is finished, the pH value of the reaction solution is adjusted to 7-7.5 with a 10% NaOH aqueous solution by mass percentage concentration, then fully washed 2-3 times with deionized water, the organic phases are combined, dried with anhydrous sodium sulfate, filtered, The filtrate was concentrated in vacuo, and the residue was subjected to 300-400 mesh silica gel column chromatography, using a mixture of ethyl acetate and chloroform at a volume ratio of 1:3 as the eluent, thereby obtaining the compound of the above formula (II), wit...
Embodiment 3
[0049]
[0050] At room temperature, add 100 mmol of the above formula (I) compound, 6 mmol of the catalyst 1-benzyl-3-methylimidazolium bromide, 150 mmol of p-nitrobenzenesulfonic acid, and 15 mmol of the above-mentioned organic phosphine ligand L1 to an appropriate amount of organic solvent DMSO and 200 mmol 2-iodoethyl methyl ether, and the temperature was raised to 80° C. and the reaction was stirred at this temperature for 4 hours.
[0051] After the reaction is finished, the pH value of the reaction solution is adjusted to 7-7.5 with a 10% NaOH aqueous solution by mass percentage concentration, then fully washed 2-3 times with deionized water, the organic phases are combined, dried with anhydrous sodium sulfate, filtered, The filtrate was concentrated in vacuo, and the residue was subjected to 300-400 mesh silica gel column chromatography, using a mixture of ethyl acetate and chloroform at a volume ratio of 1:4 as the eluent to obtain the compound of formula (II) with ...
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More