Method for preparing scutellarin
A technology of acetylation and compounds, applied in the field of drug synthesis, can solve the problems of cumbersome process, lack of raw material sources, low yield, etc., and achieve the effect of simple process, rich source, and high yield
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Embodiment 1
[0047] Step 1: Preparation of Compound II
[0048] Weigh 18.4g (0.1mol) of 3,4,5-trimethoxyphenol into a reaction vessel, add about 30ml of acetic anhydride, slowly add BF under stirring at room temperature 3 The solution was 10ml, and then slowly heated to 40° C. for 3 hours (TLC checks that the raw materials have reacted completely).
[0049]The above reaction solution was slightly cooled naturally, added with 100 ml of ethyl acetate and stirred, then placed in the refrigerator overnight, and filtered to obtain the precipitated yellow solid. Add 100ml of water and 10ml of ethanolamine to the yellow solid, stir well for 1-2 hours, and then extract the product twice with ethyl acetate, 80ml each time. The extracts were combined, washed once with water, dried over anhydrous sodium sulfate, filtered, and the solvent was evaporated under reduced pressure to obtain compound II as a light yellow oil, which could solidify after being refrigerated, dried and weighed, yield: 84%. 1 ...
Embodiment 2
[0076] Step 1: Preparation of compound II
[0077] Weigh 18.4g (0.1mol) of 3,4,5-trimethoxyphenol into a reaction vessel, add about 30ml of acetic acid, slowly add 50g of polyphosphoric acid under stirring at room temperature, then slowly heat to 80°C for 1 hour (TLC Check that the raw material has reacted completely).
[0078] Under stirring, the above reaction solution was poured into 150 ml of ice-cold water while hot, and then the product was extracted twice with ethyl acetate, 100 ml each time. The extracts were combined, washed once with water, dried over anhydrous sodium sulfate, filtered, and the solvent was distilled off under reduced pressure to obtain compound II as a light yellow oil, which could solidify after being refrigerated, dried and weighed, yield: 85%. 1 HNMR (CDCl 3):Cit.
[0079] Step 2: Preparation of compound III
[0080] Weigh 15.2g (0.10mol) of 3,4,5-trimethoxybenzoic acid and place it in a reaction flask, add 40ml of dichloromethane, 15ml of SOC...
Embodiment 3
[0103] Step 1: Preparation of compound II
[0104] Weigh 18.4g (0.1mol) of 3,4,5-trimethoxyphenol into a reaction vessel, add about 30ml of acetyl chloride, slowly add 50g of anhydrous titanium tetrachloride under stirring at room temperature, and then slowly heat to 60°C for reaction 2 hours (TLC checks that the starting material has reacted completely).
[0105] Under stirring, the above reaction solution was poured into 150 ml of ice-cold water while hot, and then the product was extracted twice with ethyl acetate, 100 ml each time. The extracts were combined, washed once with water, dried over anhydrous sodium sulfate, filtered, and the solvent was evaporated under reduced pressure to obtain compound II as a light yellow oil, which could solidify after refrigeration, dried and weighed, yield: 88%. 1 HNMR (CDCl 3 ):Cit.
[0106] Step 2: Preparation of compound III
[0107] Weigh 15.2g (0.10mol) of 3,4,5-trimethoxybenzoic acid and place it in a reaction flask, add 40ml o...
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