Method for preparing R-6-hydroxy-1-aminoindane through dynamic kinetic resolution
A dynamic kinetics, R-6- technology, which is applied in the field of dynamic kinetics splitting and preparing R-6-hydroxy-1-aminoindane, can solve the problem of splitting and preparing R-6-hydroxy-1-aminoindene, etc. problem, to achieve the effect of complete utilization of raw materials, simple operation and high optical purity
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Embodiment 1
[0007] 1. Resolution of 6-hydroxy-1-aminoindan
[0008] In a 1000ML autoclave, add 500ML toluene, 74.5G 6-hydroxy-1-aminoindan, 115.9g D-(-)-O-acetylmandelic acid, 6g Candida plicata lipase and 10g KT-02, seal the autoclave, Replace the air in the autoclave with nitrogen, then feed hydrogen into the autoclave to a pressure of 1.0MP, start stirring, and raise the temperature to 50°C for reaction; after 19 hours, take a sample and detect that 6-hydroxy-1-aminoindane is completely converted It is the acetyl compound of R-6-hydroxyl-1-aminoindane; after the reaction, the solution is concentrated and subjected to column chromatography to obtain 90.8 g of the acetyl compound of pure R-6-hydroxyl-1-aminoindane, The yield was 95.1%.
[0009] 2. Acid hydrolysis to obtain R-6-hydroxy-1-aminoindan
[0010] Take 95.5 g of the acetyl compound of R-6-hydroxy-1-aminoindane obtained by repeating the previous step several times and add it to 1000 ml of ethanol and concentrated hydrochloric a...
Embodiment 2
[0014] 1. Resolution of 6-hydroxy-1-aminoindan
[0015] In a 1000ML autoclave, add 500ML of toluene, 74.5G of 6-hydroxy-1-aminoindan, 144.9g of D-(-)-O-acetylmandelic acid, 7g of Candida plicata lipase and 13g of KT-02 in sequence, and seal the autoclave , replace the air in the autoclave with nitrogen, then pass hydrogen into the autoclave to a pressure of 1.5MP, start stirring, and raise the temperature to 70°C for reaction; after 13 hours, take a sample for detection, 6-hydroxy-1-aminoindane Completely converted into the acetyl compound of R-6-hydroxyl-1-aminoindan; after the reaction, the solution was concentrated and subjected to column chromatography to obtain 90.4 g of the acetyl compound of R-6-hydroxyl-1-aminoindan , the yield is 94.7%.
[0016] 2. Acid hydrolysis to obtain R-6-hydroxy-1-aminoindan salt
[0017] Take 95.5 g of the acetyl compound of R-6-hydroxy-1-aminoindane obtained by repeating the previous step several times and add it to a solution mixed with 10...
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