Process for preparing D-proline
A technology of proline and proline refined salt, which is applied in the direction of organic chemistry, can solve the problems of low total yield, increased consumption, and difficulty in obtaining pure products, and achieve the effect of reducing costs and usage
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[0024] The first step D-tartrate·D-proline salt preparation
[0025] Dissolve the mixture of 11.5g L-proline and 15.0g D-tartaric acid in 150.00mL organic acid, add 10-30% aliphatic aldehyde, stir at 80±5°C for 4 hours, cool to room temperature and then use Cool in an ice-water bath for 0.5 hour and filter. The solid was washed with absolute ethanol and dried to obtain 23.1 g of white crystals of D-proline D-tartrate, with a yield of 87.2%, [α] D 20 22.0°.
[0026] The crude salt was recrystallized with 95% ethanol to obtain 19.0g of refined salt with a yield of 82.3%, [α] D 20 24.0°.
[0027] Preparation of the second step D-proline
[0028] Dissolve 26.5 g of D-proline refined salt of D-tartrate obtained by the above recrystallization in methanol, slowly add ammonia gas under stirring at 20-65°C to make the solution weakly alkaline, stir at room temperature for 1 hour, and then cool to 5~ 10°C, filter and wash the solid with an appropriate amount of methanol for 1-2 t...
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