ChemicalBook CAS DataBase List N,N-Dimethylformamide dimethyl acetal

N,N-Dimethylformamide dimethyl acetal synthesis

6synthesis methods

Product Name:N,N-Dimethylformamide dimethyl acetal
CAS Number:4637-24-5
Molecular formula:C5H13NO2
Molecular Weight:119.16

124-41-4

68-12-2

4637-24-5

A method for synthesizing N,N-dimethylformamide dimethyl acetal, comprising the steps of (1) heating N,N-dimethylformamide to 70°C, mixing with dimethyl sulfate in a molar ratio of 1:1 and reacting for 4 hours after the end of dropwise addition to obtain the imine complex, and then cooling to room temperature; (2) adding solid sodium methanol to 200 solvent oil, dispersing it by ultrasonication, adjusting the temperature to 25 ℃ and maintained, dropwise addition of the imine complex, the reaction for 2 hours and then filtered, the filtrate often pressure fractionation, collection of 105-108 ℃ fraction, to obtain N,N-dimethylformamide dimethyl acetal, the yield was 75.3%, purity of 97%; wherein the molar ratio of sodium methanol to the imine complex is 1:1. The synthesis of the N,N-dimethylformamide dimethyl acetal of Example 6 is the same as that of Example 2, the The difference is that the organic solvent of this embodiment is a mixed solvent oil: D40 solvent oil, D60 solvent oil and 260 solvent oil, with a volume ratio of 2:1:1, to obtain N,N-dimethylformamide dimethyl acetal with a yield of 85.4% and a purity of 97%.

124-40-3
541 suppliers
$18.00/100ml

149-73-5 Synthesis

149-73-5
544 suppliers
$12.00/5g

4637-24-5
651 suppliers
$5.00/25g

Yield:4637-24-5 95%

Reaction Conditions:

with acetyl chloride at 20; for 12 h;Inert atmosphere;

Steps:

1-3 Example 1

(1) In an argon atmosphere, add diethylamine, acetyl chloride, and triethyl orthoacetate to the reaction vessel and mix them evenly at a molar ratio of 1:0.2:2.6;(2) Place the reaction vessel on a stirrer at room temperature and vigorously stir and react for 12 hours, and the reaction product is purified by distillation to obtain N,N-dimethylformamide dimethyl acetal with a yield of 95%

References:

CN111454231,2020,A Location in patent:Paragraph 0037-0039; 0043-0050