5-[(2R)-2-Aminopropyl]-1-[3-(benzoyloxy)propyl]-2,3-dihydro-7-carbonitrile-1H-indole synthesis

Yield:239463-72-0 99%

Reaction Conditions:

with sodium carbonate in water;ethyl acetate; for 2 h;Large scale;

Steps:

1.1; 2.1; 3.1; 4.1; 5.1; 6.1 First Step: Preparation of 5 - [(2R) -2-aminopropyl] -2,3-dihydro-1- [3- (benzoyloxy) propyl] -1H-indole-7-carbonitrile

1. 80L water was added 200L reactor, adding sodium carbonate 6.2Kg stirring to clarify;2. Add ethyl acetate 50L, stirring,10 Kg of 5 - [(2R) -2-aminopropyl] -2,3-dihydro-1- [3- (benzoyloxy) propyl] -1H-indole-7-carbonitrile tartarate was added, Stir for 2 hours;3. Let stand liquid, the aqueous phase was extracted once with 20 L of ethyl acetate, the combined organic phase;The organic phase was washed twice with 15 L of saturated brine and the organic phase was dried over anhydrous sodium sulfate for 4 hours.5. Suction filtration, desiccant was washed with ethyl acetate; the solvent was dried under reduced pressure to give an oil 7Kg,Is 5 - [(2R) -2-aminopropyl] -2,3-dihydro-1- [3- (benzoyloxy) propyl] -1H-indole-7-carbonitrile, 99%.

References:

CN106995399,2017,A Location in patent:Paragraph 0044-0049; 0079-0084; 0114-0119; 0149-0154