
7,10-Dimethoxy-10-DAB III synthesis
- Product Name:7,10-Dimethoxy-10-DAB III
- CAS Number:183133-94-0
- Molecular formula:C31H40O10
- Molecular Weight:572.64

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Yield: 89.6%
Reaction Conditions:
with dmap;caesium bromide;sodium hydride in tetrahydrofuran;N,N-dimethyl-formamide at -30; for 3 h;Temperature;Reagent/catalyst;
Steps:
1.1 (1) Preparation of 7,10 methoxy 10-DAB
Add 100 g of 10-DAB to a dry three-necked flask, dissolve in 50 mL of DMF and 150 mL of tetrahydrofuran, stir magnetically, wait for complete dissolution, add 50 g of cesium bromide, and cool to -30 ° C under ice bath conditions, and add sequentially. 10 g of sodium hydride and 1 g of DMAP were kept under low temperature conditions, 50 mL of dimethyl carbonate was added dropwise, and the reaction was carried out for 3 hours after mixing. After the TLC test showed that the reaction was completed, the reaction solution was added to a solution of 20% by mass aqueous sodium hydrogencarbonate solution in 2000 mL. After 2 hours, the kaba intermediate intermediate 7,10 methoxy 10-DAB crystal was obtained by vacuum distillation; the crystal was washed successively with ethyl acetate for several times, and dried to obtain 105 g of white crystals, and the detected content was 85.3%, and the reaction yield was obtained. It is 89.6%.
References:
Yunnan Han De Biological Co., Ltd.;Ma Huimin;Yang Qingchun;Li Yanlan;Ma Huaihu CN108003119, 2018, A Location in patent:Paragraph 0017; 0021; 0025

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183133-94-0
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