Method for preparing (S)-6-hydroxy-1-aminoindane through dynamic kinetic resolution
A dynamic dynamics and aminoindane technology, which is applied in the preparation of organic compounds, the preparation of aminohydroxyl compounds, organic chemistry, etc., to achieve the effects of simple operation, high optical purity of products, and complete utilization of raw materials
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Embodiment 1
[0007] 1. Resolution of 6-hydroxy-1-aminoindan
[0008] In a 1000ML autoclave, sequentially add 500ML toluene, 74.5G 6-hydroxy-1-aminoindan, 115.9g L-(+)-O-acetylmandelic acid, 6g Candida plicata lipase and 10g KT-02, seal Autoclave, replace the air in the autoclave with nitrogen, then pass hydrogen into the autoclave to a pressure of 1.0MP, start stirring, and raise the temperature to 55°C for reaction; after 20 hours, sample detection, 6-hydroxyl-1-amino Indane is completely converted into the acetyl compound of (S)-6-hydroxyl-1-aminoindane; after the reaction, the solution is concentrated and subjected to column chromatography to obtain pure (S)-6-hydroxyl-1-aminoindane Full acetyl compound 90.3g, yield is 94.6%.
[0009] 2. Acid hydrolysis to obtain (S)-6-hydroxy-1-aminoindan salt
[0010] Get the acetyl compound 95.5g of (S)-6-hydroxyl-1-aminoindane that repeats the previous step to make several times and join in the solution that the ethanol of 1000ml and concentrated ...
Embodiment 2
[0014] 1. Resolution of 6-hydroxy-1-aminoindan
[0015] In a 1000ML autoclave, sequentially add 500ML toluene, 74.5G 6-hydroxy-1-aminoindan, 144.9g L-(+)-O-acetylmandelic acid, 7g Candida plicata lipase and 12g KT-02, seal 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 65°C for reaction; after 15 hours, sample detection, 6-hydroxy-1-amino Indane is completely converted into the acetyl compound of (S)-6-hydroxyl-1-aminoindane; after the reaction, the solution is concentrated and subjected to column chromatography to obtain pure (S)-6-hydroxyl-1-aminoindane The full acetyl compound was 88.9g, and the yield was 93.1%.
[0016] 2. Acid hydrolysis to obtain (S)-6-hydroxy-1-aminoindan salt
[0017] Get 95.5 g of the acetyl compound of (S)-6-hydroxyl-1-aminoindane that repeats the previous step to make several times and join in the solution that the ethanol of 1000...
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