Preparation method of methyl pheophorbide-a
A technology of pheophorbide and methyl ester, which is applied in the direction of organic chemistry, can solve the problems of ecological and environmental protection hazards, low purity, low yield of target products, etc., and achieve the effect of increasing processing output and reducing emissions
Examples
Embodiment 1
[0043] Inject 3kg of chlorella into 18L of methanol, slowly add 0.9L of concentrated H 2 SO 4 , and then mixed and stirred at 22°C for 48 hours.
[0044] The excess waste material was filtered off, the filtrate was concentrated by evaporation, the residue was added to water, and neutralized with 10% NaOH to form a precipitate. Put the precipitate in the cooling box for 12 hours, separate layers, take out and remove the clear liquid, filter the remaining part through diatomaceous earth, rinse with water for 5 times, and then rinse the product with 1800ml of hexane to remove impurities. Then, the target product was washed with acetone (2100ml) and acetone: chloroform (1:1) (5000ml) mixture successively, the washing liquid was combined, evaporated and separated to obtain the target product—a methyl pheophorbide. The solid was then washed sequentially with methanol and petroleum ether and dried.
[0045] After the solid was dissolved in dichloromethane, it was purified by silic...
Embodiment 2
[0048] Inject 10kg of Spirulina platensis into 60L of methanol, slowly add 3L of concentrated H 2 SO 4 , and then mixed and stirred at room temperature for 40 hours.
[0049] The excess waste material was filtered off, the filtrate was concentrated by evaporation, the residue was added to water, and neutralized with 10% KOH to form a precipitate. Put the precipitate in the cooling box for 18 hours, separate layers, take out and remove the clear liquid, filter the remaining part through diatomaceous earth, rinse with water 10 times, and then rinse the product with 8L of hexane to remove impurities. Then, the target product was washed with acetone (9 L) and a mixture of acetone:chloroform (1:1) (20 L) successively, the washing liquid was combined, evaporated and separated to obtain the target product—a methyl pheophorbide. It was then washed sequentially with methanol and hexane, and dried.
[0050] After the solid was dissolved in chloroform, it was purified by silica gel co...
Embodiment 3
[0053] Inject 0.1kg of Spirulina platensis into 0.6L of methanol, slowly add 0.03L of concentrated H 2 SO 4 , and then mixed and stirred at 22°C for 50 hours.
[0054] The excess waste material was filtered off, the filtrate was concentrated by evaporation, the residue was added to water, and neutralized with 10% NaOH to form a precipitate. Put the precipitate in the cooling box for 24 hours, separate layers, take out and remove the clear liquid, filter the remaining part through diatomaceous earth, rinse with water for 3 times, and then rinse the product with 60ml of hexane to remove impurities. Then, the target product was washed with acetone (70ml) and acetone:chloroform (1:1) (200ml) solution successively, the washing liquid was combined, evaporated and separated to obtain the target product--a methyl pheophorbide. It was then washed sequentially with methanol and hexane, and dried.
[0055] After the solid was dissolved in dichloromethane, it was purified by silica gel...
PUM
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Description
Claims
Application Information
- IPC
- C07D487/22
- CPC
- C07D487/22
- Inventors
- 宋治国