Preparation method of erythro-aleuritic acid
A kind of technology of Lagaric acid and Su-style, which is applied in the field of synthesis of natural products, can solve the problems of preparation and property research of red-formed Lacaric acid, and achieve high conversion efficiency of raw materials, simple operation and stable reaction temperature Effect
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Embodiment 1
[0059] Embodiment 1 prepares erythro-type lacaric acid
[0060] 1. The first reflux treatment
[0061] 30.4g threo type laccarnation acid (A, 0.1 mole) and 300ml concentration are 36.5% hydrochloric acid (3.537 mole) to be placed in the round bottom flask with reflux condenser, add catalyst ST (ZnCl 2 , 0.002 moles) and mix well; then place the flask in an oil bath to heat, feed condensed water, and under stirring, carry out the first heating-reflux treatment; wherein: the molar ratio of threo-type largaeic acid to HCl It is 1:35.37 (usually 1:15-36); the molar ratio of threo-style lacaric acid to catalyst ST is 1:0.02 (usually 1:0.001-0.070); the temperature of the first heating-reflux treatment is (100±1)°C (usually the temperature range for the first heating-reflux treatment is (90-100)±1)°C;
[0062] After the first heating-reflux treatment for 10h (usually 5-12h), cool to room temperature, suction filter, and wash the filter residue with deionized water until there is n...
Embodiment 2
[0087] 1. The first reflux treatment
[0088] In addition to the molar ratio of threo-style lactoic acid to HCl is 1:15 (usually 1:15-36); the molar ratio of threo-style lactoic acid to catalyst ST is 1:0.07; the first heating-reflux treatment The temperature is (90±1)°C (the temperature range of the first heating-reflux treatment is usually (90-100)±1)°C); except for the first heating-reflux treatment for 12h, the rest are the same as in Example 1. 1 is the same. The preparation yielded 22.6 g of intermediate IM.
[0089] 2. The second heating - reflux treatment
[0090] Except that the mass percent concentration of the NaOH aqueous solution is 5%; the temperature of the second heating-reflux treatment is (90±1)° C., the rest is the same as step 2 of Example 1.
[0091] 3. Acid analysis treatment
[0092] Except heating for the second time-reflux treatment 36h (being generally 25-36h); The mass percent concentration of the dilute hydrochloric acid that adds in the reactio...
Embodiment 3
[0094] 1. The first reflux treatment
[0095] Except that the molar ratio of threo-style lacaric acid to HCl is 1:30 (usually 1:15-36); the molar ratio of threo-style lactalic acid to catalyst ST is 1:0.001; the first heating-reflux treatment The temperature is (100±1)°C (the temperature range of the first heating-reflux treatment is usually (90-100)±1)°C); except for the first heating-reflux treatment for 5h, the rest are the same as in Example 1. 1 is the same. The preparation yielded 26.5 g of intermediate IM.
[0096] 2. The second heating - reflux treatment
[0097] Except that the mass percent concentration of the NaOH aqueous solution is 8%; the temperature of the first heating-reflux treatment is (100±1)° C., the rest are the same as step 2 of Example 1.
[0098] 3. Acid analysis treatment
[0099] Except heating for the second time-reflux treatment 25h (being generally 25-36h); The mass percent concentration of the dilute hydrochloric acid that adds in the reactio...
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