Production of hair orchid
一种毛兰素、化合物的技术，应用在毛兰素的制备领域，能够解决技术要求高、不利大规模生产、原料石斛来源紧缺等问题
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Embodiment 1
[0077] [embodiment 1] the chemical synthesis of Erianin
[0078] 1. Preparation of 3,4,5-trimethoxybenzyl alcohol
[0079] In a 250ml three-necked flask, add 15g (76.45mmol) of 3,4,5-trimethoxybenzaldehyde, 200ml of absolute ethanol, heat to 40°C to dissolve, then add 1.48g (38.23mmol) of sodium borohydride, and heat to reflux After 45min, TLC detection, after the reaction is complete, cool to room temperature, add 10ml (555.8mmol) of deionized water, after quenching, filter with suction, wash the filter residue with 20ml of absolute ethanol, after combining the filtrates, concentrate to dryness with a rotary evaporator , add 100ml of dichloromethane to dissolve, wash with 2N sodium hydroxide solution 50ml x 2, then wash with deionized water 50ml x 2, add appropriate amount of anhydrous magnesium sulfate to dry overnight. Filter, wash the filter residue with 20 ml of dichloromethane, combine the filtrates, and concentrate to dryness with a rotary evaporator to obtain 3,4,5-tr...
Embodiment 2
[0107] [embodiment 2] the chemical synthesis of Erianin
[0108] 1. Bromination of 3,4,5-trimethoxytoluene
[0109] Add 10mmol of 3,4,5-trimethoxytoluene into a 50ml three-necked flask, add 20ml of carbon tetrachloride, heat and stir to an oil bath of 82-84°C, reflux the reaction solution, and then add 10mmol of N-bromo A mixture of substituted succinimide (NBS) and 0.5 mmol benzoyl peroxide (BPO), the addition time is about 10 minutes, after the addition, continue to stir and react for 20 minutes, and then filter. The filtrate was washed with water and saturated sodium chloride solution, dried over anhydrous magnesium sulfate and filtered. The filtrate was evaporated to dryness and passed through a column to collect the most polar component to obtain the product 3,4,5-trimethoxybenzyl bromide.
[0110] 2. Reaction with triethyl phosphite
[0111] 10mmol of 3,4,5-trimethoxybenzyl bromide, 50mmol of triethyl phosphite, and 40ml of toluene were stirred and refluxed for 12hr. ...
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