Preparation of R-6-methoxy-1-aminoindane through resolution

[0007] 1. Resolution of 6-methoxy-1-aminoindan

[0008] In a 1000ML autoclave, add 500ML toluene, 81.6G6-methoxy-1-aminoindan, 115.9gD-(-)-O-acetylmandelic acid, 5g Candida plicata lipase and 10gKT-02, seal the high pressure In the 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 50°C for reaction; after 18 hours, take a sample for detection, 6-methoxy-1-amino Indane is completely converted into the acetyl compound of R-6-methoxy-1-aminoindane; after the reaction, the solution is concentrated and column chromatographed to obtain pure R-6-methoxy-1-aminoindane Full acetyl compound 97.5g, yield is 95.1%.

[0009] 2. Acid hydrolysis to obtain R-6-methoxy-1-aminoindan

[0010] Get 102.6g of the acetyl compound 102.6g of the R-6-methoxy-1-aminoindane that repeats several times to be made in the previous step and join in the solution that the ethanol of 1000ml and c...

[0014] 1. Resolution of 6-methoxy-1-aminoindan

[0015] In a 1000ML autoclave, sequentially add 500ML toluene, 81.6G6-methoxy-1-aminoindan, 144.9gD-(-)-O-acetylmandelic acid, 7g Candida plicata lipase and 12gKT-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 70°C for reaction; after 14 hours, sample detection, 6-methoxy-1 -Aminoindane is completely converted into an acetyl compound of R-6-methoxy-1-aminoindane; after the reaction, the solution is concentrated and column chromatography is obtained to obtain R-6-methoxy-1-amino The acetyl compound of indane was 97.1g, and the yield was 94.7%.

[0016] 2. Acid hydrolysis to obtain R-6-methoxy-1-aminoindan salt

[0017] Get 102.6 g of the acetyl compound of R-6-methoxy-1-aminoindane obtained by repeating the previous step several times and add it to the solution mixed with 1000 ml of ethanol and concentr...