Dimethylformamide → NSC650609

Temperature

25 °C

Into a 5 L round-bottom flask fitted with a thermometer, a nitrogen-introducing tube, and a stirrer were charged 254 g of pentaerythritol and 2,500 g of N,N-dimethylformamide, and they were heated and dissolved at 80° C. After cooling to 25° C., 195 g of 2,2-dimethoxypropane and 3.6 g of p-toluenesulfonic acid monohydrate were placed therein and, with introduction of nitrogen thereinto, a reaction was carried out at 25° C. without further treatment. Neutralization was performed by adding 9.5 g of triethylamine and the reaction solution was concentrated. After concentration, the resulting powder was dispersed in 1 kg of hexane, followed by stirring and filtration. The hexane-washing step was repeated four times. The resulting cake was dissolved in 1 kg of ethyl acetate at 50° C. and, after insoluble matter was filtrated, 250 g of Kyoward 200B was added to the filtrate and adsorption treatment was performed at 50° C. for 1 hour. The filtrate was concentrated to obtain 2,2-dimethyl-5,5-bis(hydroxymethyl)-1,3-dioxane.

1. customInto a 5 L round-bottom flask fitted with a thermometer
2. additiona nitrogen-introducing tube, and a stirrer
3. temperaturewere heated
4. dissolutiondissolved at 80° C
5. customwas carried out at 25° C. without further treatment
6. concentrationthe reaction solution was concentrated
7. concentrationAfter concentration
8. additionthe resulting powder was dispersed in 1 kg of hexane
9. filtrationfiltration
10. washThe hexane-washing step
11. dissolutionThe resulting cake was dissolved in 1 kg of ethyl acetate at 50° C.
12. filtrationafter insoluble matter was filtrated
13. addition250 g of Kyoward 200B was added to the filtrate and adsorption treatment
14. concentrationThe filtrate was concentrated

ORD record

ord-27927eca114045c19890a4dc80728780

Source dataset

uspto-grants-2015_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09029568B2