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ChemicalBook CAS DataBase List Dinoprost tromethamine

Dinoprost tromethamine synthesis

10synthesis methods
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Yield:38562-01-5 92.5%

Reaction Conditions:

Stage #1: dinoprost in acetonitrile at 43 - 47; for 0.25 h;
Stage #2: 2-amino-2-hydroxymethyl-1,3-propanediol in water;acetonitrile at 53 - 57; for 0.0833333 h;

Steps:



The oil of 150 g of prostaglandin F2α (formula 6) was mixed with 5 L of acetonitrile and heated to dissolve. The temperature was controlled at 43 to 47 ° C and stirred for 15 min.And then filtered hot to obtain the filtrate, and then washed with acetonitrile, the total volume of acetonitrile to 21L, combined filtrate, and stir for 5min or so,In the course of stirring, to the filtrate by adding tromethamine solution, tromethamine solution by 49.2g of butyral trioxide and 90ml of water, and heated to 53 ~ 57 holding temperature for 5min, after the addition of crystallization Precipitation, add to continue after mixing 18 ~ 24h,And then natural cooling to room temperature, filtration, washing with acetonitrile crystallization 3 times, each 100ml, placed in a dry phosphorus pentahydrate drying vacuum to constant weight, generally need more than 5h, get tromethamine prostaglandin F2α ( 7) of about 180 g in 89% yield.

References:

CN106810484,2017,A Location in patent:Paragraph 0025

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