Synthetic method for (2R)-3-bromo-2-hydroxy-2-methylpropionic acid
A technology of methylpropionic acid and synthesis method, applied in the directions of organic chemistry method, carboxylate/lactone preparation, organic chemistry, etc., can solve the problems of long supply time, unstable quality, complicated synthesis process, etc. Simple, easy to operate, high-yield effect
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Embodiment 1
[0020] A synthetic method for (2R)-3-bromo-2-hydroxyl-2-methylpropionic acid, comprising the following steps:
[0021] (1) Preparation of methacryloyl-D-proline: at 10°C, D-proline, NaOH, MTBE and resorcinol were mixed and stirred evenly, then methacryloyl chloride was added dropwise, and Stir evenly at 20°C, let stand to separate layers, and take the upper organic phase to obtain methacryloyl-D-proline;
[0022] Then add HCl dropwise to the lower aqueous phase at 10-20°C while stirring, then add ethyl acetate, separate the liquid, and collect the organic phase; the mass-volume ratio of D-proline, HCl and ethyl acetate is: 8kg: 8.8L: 40L; then add resorcinol to the above organic phase, concentrate to 2.5 volumes at 37°C, then add toluene for the first time, concentrate to 2.5 volumes at 37°C, then add the second Secondary toluene, stir evenly, be cooled to 12 ℃, use toluene to wash the filter cake after filtering; The mass volume ratio of described D-proline, resorcinol, tolu...
Embodiment 2
[0043] A method for synthesizing (2R)-3-bromo-2-hydroxy-2-methylpropionic acid, comprising the following steps;
[0044] (1) Preparation of methacryloyl-D-proline: at 5°C, D-proline, NaOH, MTBE and resorcinol were mixed and stirred evenly, then methacryloyl chloride was added dropwise, and Stir evenly at 15°C, let stand to separate layers, and take the upper organic phase to obtain methacryloyl-D-proline;
[0045] The mass-to-volume ratio of D-proline, NaOH, MTBE, resorcinol, and methacryloyl chloride: 5kg:5kg:20L:0.5g:7kg;
[0046] In the step (1), add HCl dropwise to the separated lower aqueous phase at 10°C while stirring, then add ethyl acetate, separate the liquids, and collect the organic phase; the D-proline, HCl and The mass volume ratio of ethyl acetate is: 5kg:5L:30L.
[0047] Add resorcinol to the above organic phase, concentrate to 2 volumes at 35°C, then add toluene for the first time, concentrate to 2 volumes at 35°C, then add toluene for the second time, stir ...
Embodiment 3
[0054] A method for synthesizing (2R)-3-bromo-2-hydroxy-2-methylpropionic acid, comprising the following steps;
[0055] (1) Preparation of methacryloyl-D-proline: at 5-20°C, mix and stir D-proline, NaOH, MTBE and resorcinol evenly, then add methacryloyl chloride dropwise, And at 25°C, stir evenly, let stand to separate layers, take the upper organic phase to obtain methacryloyl-D-proline;
[0056] The mass-to-volume ratio of D-proline, NaOH, MTBE, resorcinol, and methacryloyl chloride: 9kg:7kg:28L:1g:9kg;
[0057] In the step (1), add HCl dropwise to the separated lower aqueous phase at 10-20°C while stirring, then add ethyl acetate, separate the liquids, and collect the organic phase; the D-proline, The mass volume ratio of HCl and ethyl acetate is: 9kg:10L:45L.
[0058] Then add resorcinol to the above organic phase, concentrate to 3 volumes at 40°C, then add the first toluene, concentrate to 3 volumes at 40°C, then add the second toluene, stir evenly, Cool to 15°C, filt...
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