N-Methyl-D-glucamine → N-(2-ethylhexyloxycarbonyl)-N-methyl-D-glucamine

温度

5 °C

In a reactor, 117 g (0.6 mol) of N-methyl-D-glucamine were dissolved in a mixture of 800 ml of water and 400 ml of tetrahydrofuran, and 201.6 g (2.4 mol) of sodium hydrogen carbonate were then dispersed. While the temperature of the reaction mixture was maintained at 5° C., 115.6 g (0.6 mol) of 2-ethylhexyl chloroformate were added dropwise, and the mixture was then allowed to react for 3 hours with stirring at 5° C. and left standing overnight at room temperature. The reaction mixture was then filtered and concentrated; the pasty residue obtained was dissolved in 2 liters of acetone and then filtered after cooling to 5° C. The crystallized product collected was dried. 105 g (50% yield) of N-(2-ethylhexyloxycarbonyl)-N-methyl-D-glucamine, the melting point of which is 74° C., were obtained.

1. additionwere then dispersed
2. customto react for 3 hours
3. waitleft
4. filtrationThe reaction mixture was then filtered
5. concentrationconcentrated
6. customthe pasty residue obtained
7. filtrationfiltered
8. temperatureafter cooling to 5° C
9. customThe crystallized product collected
10. customwas dried

ORDレコード

ord-774e7cff87054fc098cc64b519894e8d

出典データセット

uspto-grants-1996_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US05587169