Roxatidine synthesis
- Product Name:Roxatidine
- CAS Number:78273-80-0
- Molecular formula:C17H26N2O3
- Molecular Weight:306.4
Yield:78273-80-0 93.1%
Reaction Conditions:
at 80 - 165;
Steps:
7 Example 7: Preparation of Roxatitin Hemisoxalate (Compound 9)
450 g (1.812 mol) of compound A (prepared in Example 6) was added to the reaction flask, heated to 80° C. and added in portions.150g (1.972mol) glycolic acid, continue to heat up to a temperature of 160 ~ 165 °C, about 4 ~ 5hr reaction is completed,Cool down to about 70° C., add 800 g of ethyl acetate to the reaction solution, and stir to dissolve the reactants, using 45 g of carbon.The aqueous solution of potassium acid is thoroughly stirred and washed, allowed to stand, and the liquid is separated. The aqueous phase is extracted once with 300 g of ethyl acetate.Combine the organic phase with an aqueous solution containing 50 g of sodium chlorideWash once, separate the organic phase, add anhydrous sodium sulfate and activated carbon, dry and decolorize with stirring, and filter.The filtrate was collected and the dry solvent was concentrated to give (Compound 8) 517 g of an oil (theoretical amount: 555.16 g); Yield: 93.1%All 517 g (1.687 mol) of compound 8 obtained above were dissolved with 1500 g of absolute ethanol.106 g (0.840 mol) of oxalic acid dihydrate was added. After the addition was completed, the mixture was heated to reflux for about 1 hr under stirring, cooled to 0 to 5° C., stirred for about 4 hr, and filtered to obtain about 600 g of a white solid (Compound 9). Wet weight, crude product). Purification: The above-obtained 600 g of wet product is recrystallized with 2500 g of an aqueous 85% ethanol solution.The purified compound 9 was 423 g in dry weight (theoretical amount: 636.72 g; calculated as 450 g of compound A); yield: 66.4%.
References:
Inner Mongolia Jingdong Pharmaceutical Co., LTD.;Guo, Rong Yao;Wang, Xiao Feng;Inner Mongolia Jingdong Pharmaceutical Co., Ltd.;Guo Rongyao;Wang Xiaofeng CN107698538, 2018, A Location in patent:Paragraph 0070-0073
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