A kind of synthetic method of (r)-3-aminobutanol
A technology of aminobutanol and aminobutyric acid, applied in the field of medicine and chemical industry, can solve the problems of complex operation, high cost and low yield
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Embodiment 1
[0021] Under the protection of nitrogen, 90 g of sodium borohydride and 100 g of (R)-3-aminobutyric acid were added to reaction flask 1, and then 1 L of tetrahydrofuran was added, cooled with ice water, and set aside. 200 mL of tetrahydrofuran was added to reaction flask 2, cooled in an ice-water bath, and concentrated sulfuric acid was slowly added dropwise to reaction flask 2 to prepare a tetrahydrofuran solution of sulfuric acid. The tetrahydrofuran sulfate solution in reaction flask 2 was slowly added dropwise into reaction flask 1, and the tail gas was absorbed with sodium hydroxide solution. After the dropwise addition, the temperature was raised to 60° C. to react until the raw materials disappeared. Add sodium hydroxide solution to quench the reaction, let stand to separate layers, and distill the organic phase to recover tetrahydrofuran; extract the aqueous phase with chloroform, combine the extracts, dry with anhydrous sodium sulfate, filter, and concentrate to obtai...
Embodiment 2
[0023] Under nitrogen protection, 120 g of sodium borohydride and 124 g of (R)-3-aminobutyric acid were added to the reaction flask, 1.5 L of tetrahydrofuran was added, and cooled with ice water. Slowly drop 506g of trifluoroacetic acid into the reaction flask, and absorb the tail gas with sodium hydroxide solution. After the dropwise addition, the temperature was raised to 20°C to react until the raw materials disappeared. Sodium hydroxide solution was added to quench the reaction, the layers were separated, and the organic phase was distilled to recover tetrahydrofuran. The aqueous phase was extracted with chloroform, and the extracts were combined, dried over anhydrous sodium sulfate, filtered, and concentrated to obtain a crude product, which was distilled under reduced pressure to obtain the product. Yield: 84.3%, purity: 99.5%, ee: 99.6%.
Embodiment 3
[0025] Under the protection of nitrogen, 45g of sodium borohydride and 60g of (R)-3-aminobutyric acid were added to reaction flask 1, 1L of tetrahydrofuran was added, cooled with ice water, and set aside. Ethylene glycol dimethyl ether was added to the reaction flask 2, cooled in an ice-water bath, and 62 g of concentrated sulfuric acid was slowly added dropwise to the reaction flask 2 to prepare a ethylene glycol dimethyl ether solution of sulfuric acid. The sulfuric acid ethylene glycol dimethyl ether solution in reaction flask 2 was slowly added dropwise to reaction flask 1, and the tail gas was absorbed with sodium hydroxide solution. After the dropwise addition was completed, the temperature was raised to react until the raw materials disappeared. Sodium hydroxide solution was added to quench the reaction, the layers were separated, and the organic phase was distilled to recover tetrahydrofuran. The aqueous phase was extracted with chloroform, and the extracts were combi...
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