4,4-Diethoxy-N,N-dimethyl-1-butanamine synthesis
- Product Name:4,4-Diethoxy-N,N-dimethyl-1-butanamine
- CAS Number:1116-77-4
- Molecular formula:C10H23NO2
- Molecular Weight:189.3
Yield:1116-77-4 75.8%
Reaction Conditions:
with iodine;magnesium in benzene for 3.25 - 4.33333 h;Heating / reflux;
Steps:
4 Preparation of the Grignard reagent and the compound of the formula-I where [R'=] [R2= ME AND R3=ET]
Into a 2L four-necked round bottom flask was charged magnesium turnings (25gr) under nitrogen atmosphere. Benzene [(50ML),] the above benzene solution [(50ML),] triethyl orthoformate (20gr), and a small crystal of iodine were added to the reaction flask and slowly heated to reflux temperature. Within 15-20min of refluxing period, a vigorous reaction took place indicating the initiation of Grignard reaction. Remaining quantity of benzene solution and triethyl orthoformate of the [FORMULA-XVII] where [R3 = R5] = Et (174gr) were separately taken into two addition funnels and slowly added in 3-4hrs period to the reaction mixture under reflux temperature. The reaction mass was cooled to [25°C] and filtered through celite pad. The cake was washed with benzene [(100ML).] Benzene was removed from the reaction mass using 20cm Vigroux column at atmospheric pressure. The residue was distilled under mild vaccum keeping mass temperature below [100°C] to get the excess triethyl orthoformate (60gr). Finally, [4- (N,] N- dimethylamino)-butyraldehyde diethyl acetal was distilled under vaccum to get 125gr (75.8%) as colourless liquid. B. p.: [140-150°C/15-20MM.]
References:
NATCO PHARMA LIMITED WO2003/101931, 2003, A2 Location in patent:Page 14-15
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1116-77-4
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6346-09-4
153 suppliers
$21.00/1g
1116-77-4
302 suppliers
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