864750-70-9Relevant articles and documents
Preparation method of revefenacin
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, (2021/07/17)
The invention discloses a preparation method of revefenacin. The preparation method comprises the following steps: (1) carrying out a reductive amination reaction on methyl p-formylbenzoate as shown in a formula I and a compound as shown in a formula II to obtain a compound as shown in a formula III; (2) carrying out a hydrolysis reaction on the compound as shown in the formula III and a sodium hydroxide solution to obtain a compound as shown in a formula IV; (3) carrying out a condensation reaction on the compound as shown in the formula IV, a compound as shown in a formula V, 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride and 1-hydroxybenzotriazole to obtain a compound as shown in a formula VI; (4) carrying out an acid hydrolysis reaction on the compound as shown in the formula VI and a hydrochloric acid solution to obtain a compound as shown in a formula VII; and (5) carrying out a reductive amination reaction on the methyl p-formylbenzoate as shown in the formula VII and a compound as shown in a formula VIII to obtain revefenacin as shown in a formula IX. According to the method provided by the invention, a synthesis route is shortened, a Pd/C hydrogenation high-pressure protecting group removal process is avoided, and the method has the advantages of milder and safer reaction conditions and the like.
New rafenacin intermediate, active electrophilic building block thereof and new preparation method of rafenacin
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, (2021/04/26)
The invention provides a new rafenacin intermediate, an active electrophilic building block thereof and a new preparation method of rafenacin. The new rafenacin intermediate shown as the formula (II) is prepared by sequentially reacting N-methylethanolamine with a compound shown as a formula (III) and a compound shown as a formula (V), and the new rafenacin intermediate shown as the formula (II) is used for activating hydroxyl to prepare an active electrophilic block shown as a formula (VI) and then reacts with a compound shown as a formula (VII) to obtain the rafenacin shown as the formula (I). The synthetic route provided by the invention has the advantages of short reaction steps, low raw material cost, simple reaction operation, mild conditions, high conversion rate, high selectivity and convenient post-treatment, and is more suitable for industrial production.
PROCESS FOR PREPARING A BIPHENYL-2-YLCARBAMIC ACID
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, (2012/02/01)
The invention provides a process of preparing an intermediate useful in the synthesis of biphenyl-2-ylcarbamic acid 1-(2-{[4-(4-carbamoylpiperidin-1-ylmethyl)benzoyl]methylamino}ethyl)piperidin-4-yl ester, and a process of preparing a crystalline freebase of the ester.