Butanedioic acid, compd. with (+)-N,N-dimethyl-2-[1-phenyl-1-(2-pyridinyl)ethoxy]ethanamine (1:1) (9CI) synthesis
- Product Name:Butanedioic acid, compd. with (+)-N,N-dimethyl-2-[1-phenyl-1-(2-pyridinyl)ethoxy]ethanamine (1:1) (9CI)
- CAS Number:76216-25-6
- Molecular formula:C21H28N2O5
- Molecular Weight:388.46
Yield:76216-25-6 93.5%
Reaction Conditions:
with pyrographite in ethyl acetate at 60;Temperature;Solvent;
Steps:
1.2; 2.2; 3.2; 1; 2
(2) In a 1000 ml three-necked flask, dissolve 124.5 g (0.46 mmol) of doxylamine obtained in step (1) in 300 g of ethyl acetate, heat up to 60 ° C, and add 54.3 g (0.46 mmol) of succinic acid. After adding medicinal activated carbon for decolorization and filtration, slowly reduce the temperature to 5 ° C, and precipitate a large amount of white solids. Stir and crystallize for 1 hour, suction filter, rinse with pre-cooled ethyl acetate, and vacuum dry at 60 ° C.166g of doxylamine succinate was obtained with a yield of 93.5%,Melting point is 103.7 to 104.8 ° C.HPLC purity 99.85%,GC purity was 99.86%.
References:
CN110498764,2019,A Location in patent:Paragraph 0056; 0058; 0059; 0061; 0062; 0064-0068
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