60050-48-8Relevant articles and documents
Preparation method of 3-aminopropanol or 3-aminopropionic acid derivative
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Paragraph 0150-0154; 0157, (2018/10/11)
The invention provides a preparation method of an optically active 3-aminopropanol or 3-aminopropionic acid derivative, and belongs to the technical field of organic synthesis. A compound having a structure as shown in a formula II and a formula III is used as a raw material, and the optically active 3-aminopropanol or 3-aminopropionic acid derivative is obtained through four basic steps, namely dehydration condensation, hydrogenation reduction, reduction and hydrolysis. The raw materials adopted in the preparation method are easy to obtain and low in cost; as a chiral phosphine-transitional metal catalyst is used in the hydrogenation reduction reaction, the optically active 3-aminopropanol or 3-aminopropionic acid derivative is efficient, high in selectivity, low in cost and suitable forlarge-scale production. Compared with existing chemical resolution and chiral introduction, the asymmetric hydrogenation synthesis method provided by the invention only produces one chiral product, ishigh in yield, and has relatively high advantages in economy and raw material utilization rate.
The optically pure 3-amino-1-butanol method for the preparation of
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Paragraph 0056; 0057, (2016/12/22)
The invention provides a method for preparing optically pure 3-amino-1-butanol. The method comprises the following steps: reacting benzamide and acetoacetate under the catalytic action of p-toluenesulfonic acid to generate 3-benzamido-2-crotonate; carrying out catalytic hydrogenation reaction by using a chiral rhodium-diphosphine ligand compound as an asymmetric hydrogenation catalyst to generate 3(R)/(S)-benzamidobutyrate at high selectivity; reducing ester carbonyl group with hydroborate to generate 3(R)/(S)-benzamido-1-butanol; and finally, carrying out hydrolysis and benzoyl removal with concentrated hydrochloric acid to obtain the optically pure 3(R)/(S)-amino-1-butanol. The method has the advantages of cheap and accessible raw materials, simple technical operation, no need of resolution, high yield, low cost, environment friendliness and high optical purity of the product, and is more suitable for industrial production.
A 3 (R) / (S)-amino-1-butanol method for the preparation of
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Paragraph 0059; 0060, (2017/01/17)
The invention provides a method for preparing 3(R)/(S)-amidogen-1-butanol. The method comprises the steps that firstly, benzamide reacts with acetoacetic ester under the catalyzing action of p-toluenesulfonic acid, so that 3-benzamido-2-butene acid ester is generated; secondly, catalytic hydrogenation is conducted by using a chiral rhodium-diphosphine ligand compound as a catalyst for enantioselective hydrogenation, so that 3(R)/(S)-benzamide butyrate is generated highly selectively; thirdly, benzoyl is removed by means of mixed solvent of concentrated hydrochloric acid and alcohol, so that 3(R)/(S)-amino-crotonic acid ester hydrochloride is generated; finally, optically pure 3(R)/(S)-amidogen-1-butanol is obtained after ester carbonyl is reduced by means of hydronoron. According to the method, the raw materials are low in cost and easy to obtain, the technological operation is easy and convenient, resolution is not needed, the yield is high, cost is low, environmental friendliness is achieved, the optical purity of product is high, and the method is more suitable for industrial production.
