Isobutyric acid D7 synthesis method and isobutyric acid D6 synthesis method
A synthesis method and technology of isobutyric acid, applied in chemical instruments and methods, organic chemistry methods, carboxylate preparation, etc., can solve complex purification, the reaction involves many strong acids and bases, and the yield of isobutyric acid D6 is low, etc. problems, to achieve the effect of simple post-processing, short synthesis steps, and short routes
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0026] The synthetic method of embodiment 1 isobutyric acid D7
[0027] The synthetic route is as follows:
[0028]
[0029] In a 250 ml three-necked flask, add 4.12 g (169 mmol) of magnesium chips and 80 ml of anhydrous tetrahydrofuran, replace with nitrogen three times, add a little 20 g of 2-bromopropane-D7 (154 mmol) dropwise, heat to initiate the reaction, and wait for the Grignard reaction to initiate Finally, slowly add the remaining 2-bromopropane-D7 dropwise. After the completion, the reaction system continues to reflux for half an hour. After cooling the system in an ice bath, carbon dioxide gas is introduced under stirring. After the reaction is completed, most of the solvent is evaporated, and the remaining mixture is added to 40 milliliters of water, 60 milliliters of 3M hydrochloric acid solution was slowly added dropwise under ice bath, after completion, the aqueous phase was extracted with dichloromethane, the organic phases were combined, dried over anhydro...
Embodiment 2
[0030] The synthetic method of embodiment 2 isobutyric acid D6
[0031] The synthetic route is as follows:
[0032]
[0033] Dissolve 7 g of isobutyric acid-D7 (74 mmol) in aqueous sodium hydroxide solution (8.84 g (221 mmol) of sodium hydroxide, 80 ml (4.4 mol) of water) and place it in an autoclave with the temperature set at 180 °C and the rotation speed Set at 450 rpm, reacted for 40 hours, cooled in an ice bath, slowly added concentrated hydrochloric acid dropwise to adjust pH = 1, extracted several times with dichloromethane, combined organic phases, dried over anhydrous sodium sulfate, and distilled off DCM to obtain 6.5 g of crude product , Distilled under reduced pressure to obtain 5.5 g colorless transparent liquid, namely isobutyric acid D6, yield 78.6%. The HNMR result of the obtained product is as follows figure 1 As shown, the product is shown to be isobutyric acid D6.
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More