Reference of 758-96-3, A common heterocyclic compound, 758-96-3, name is N,N-Dimethylpropionamide, molecular formula is C5H11NO, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
Step alb: compound A5 (3-(3-methoxyphenyl)-N,N,2-trimethyl-3-oxopropanamide)To 2,2,6,6-tetramethylpiperidine (17.5 g, 125 mmol) in 50 ml dry THF were added dropwise 72 ml (115 mmol) of a n-buthyllithium solution in n-hexane (1.6 M) at -30C. After 30 minutes of stirring, 5.0 g (50 mmol) Nu,Nu-dimethylpropionamide (A1) (dissolved in 50 mL dry THF) were added and the mixture was cooled to -70C and stirred for 1 h at this temperature. 22.5 g (125 mmol) ethyl-3-methoxybenzoate (dissolved in 30 mL dry THF) were slowly added dropwise and the resulting mixture was stirred for another 2 h at -70C. After the mixture had been allowed to warm to RT, it was hydrolyzed by employing a diluted aqueous solution of HCI (36 mL). The mixture was then washed with diethyl ether several times. The combined organic layers were dried over MgS04. The organic solvents were evaporated under reduced pressure and the remaining residue was dried in vacuo. CC (eluent: n-hexane/ethyl acetate (1 :4)) yielded 6.5 g (55%) of A5 in form of a colorless oil.
The synthetic route of 758-96-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; GRUeNENTHAL GMBH; BUSCHMANN, Helmut, Heinrich; HOLENZ, Joerg; WO2011/157390; (2011); A2;,
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