Method for preparing nitidine chloride from total alkali extract of zanthoxylum nitidum stems and branches
A technology of chlorinating limpet base and limpet, which is applied in organic chemistry and other fields, can solve the problems of large production consumption, and achieve the effect of fast separation speed and simple operation
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Embodiment 1
[0020] Take 0.5 kg of the stems and branches of limping needles, crush them into coarse powder, add 4.0 kg of 95% ethanol to reflux and extract twice, each time for 2 hours, combine the filtrates, recover the ethanol, concentrate to a thick paste, and obtain the total alkali extraction of the stems and branches of limping needles Compound 14.2g.
[0021] Take 14.2g of the total alkali extract of the above-mentioned stems and branches of Liangmianzhen, add 28.4g of methanol to dissolve, add 28.4g of column chromatography silica gel to mix the sample, mix well, evaporate to dryness, grind to powder, put it in the chromatography column, and mix it with acetic acid Ethyl-methanol is eluted, and the volume ratio of ethyl acetate and methanol is 8:2; According to total alkali extract quality: eluent volume=1g:20ml ratio collects eluent, to each part of eluent collected TLC was used to identify and track observations, select the eluents containing chlorinated amphetine, combine them,...
Embodiment 2
[0023] Take 1.0kg of the stems and branches of the double-sided needles, crush them into coarse powder, add 10.0kg of 95% ethanol to reflux extraction for 3 times, each time for 1 hour, combine the filtrates, recover the ethanol, concentrate to a thick paste, and obtain the total alkali extraction of the stems and branches of the double-sided needles Compound 25.3g.
[0024] Take 25.3g of the total alkali extract of the above-mentioned stems and branches of Liangmianzhen, add 75.9g of methanol to dissolve, add 75.9g of column chromatography silica gel to mix the sample, mix well, evaporate to dryness, grind to powder, put it in the chromatography column, and mix it with acetic acid Ethyl-methanol is eluted, and the volume ratio of ethyl acetate and methanol is 9:1, and according to total alkali extract quality: eluent volume=1g:20ml ratio collects eluent, to each part of eluent collected Adopt thin-layer identification and follow-up observation, select the eluent containing am...
Embodiment 3
[0026] Take 2.0kg of stems and branches of limping needles, crush them into coarse powder, add 24.0kg of 95% ethanol to reflux and extract once for 3 hours each time, combine the filtrates, recover ethanol, concentrate to a thick paste, and obtain the total alkali extraction of limping needles stems and branches Compound 51.4g.
[0027] Take 51.4g of the total alkali extract of the above-mentioned stems and branches of Liangmianzhen, add 304.2g of methanol to dissolve, add 304.2g of column chromatography silica gel to mix the sample, mix well, evaporate to dryness, grind to powder, put it in the chromatography column, and mix it with acetic acid Ethyl-methanol is eluted, and the volume ratio of ethyl acetate and methanol is 7:3, and according to total alkali extract quality: eluent volume=1g:20ml ratio collects eluent, to each part of eluent collected TLC was used to identify and track observations, select the eluents containing amphetine chloride, combine them, concentrate to...
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