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ChemicalBook CAS DataBase List (S)-(-)-3-(Benzoylthio)-2-methylpropanoic acid
72679-02-8

(S)-(-)-3-(Benzoylthio)-2-methylpropanoic acid synthesis

2synthesis methods
-

Yield:72679-02-8 71.9%

Reaction Conditions:

with sodium hydroxide in water;Inert atmosphere;

Steps:

1 Example 1

Under nitrogen protection, 21.5 g of sodium hydroxide, 90 mL of drinking water and 0.4 g of zinc powder were sequentially added to the three-necked flask, and the temperature was lowered to 0 ° C, and 20 g of S-(-)-3-acetylthio-2-methylpropionic acid was slowly added dropwise, and heat preservation reaction for 3h. After the reaction was completed, the pH was adjusted to 9.0 with concentrated hydrochloric acid. The temperature of the feed liquid was controlled to 15 ° C, and 20 g of benzoyl chloride and 36 mL of a 4 mol/L aqueous sodium hydroxide solution were added dropwise. After completion of the reaction, pΗ = 2.0 was adjusted with concentrated hydrochloric acid, and extracted with 80 mL of ethyl acetate. After layering, 120 mL of n-heptane was added to the ethyl acetate layer, and the mixture was stirred and crystallizated for 4 hours, filtered, and dried to give S-(-)-benzoyl thio-2-methylpropionic acid, yield: 71.9%, HPLC: purity: 99.90%, optical purity: 99.2%.

References:

CN109651218,2019,A Location in patent:Paragraph 0020; 0021

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