Methanol → Methyl acrylamidoglycolate methyl ether

Temperatur

40 °C

To a three-necked flask equipped with a stirrer and an extractor filled with a molecular sieve drying agent was added 300 parts acrylamidoglycolic acid, 3000 parts methanol, 0.05 parts phenothiazine, 4.5 parts 98% sulfuric acid and 200 parts chloroform. The mixture was heated to reflux and the distillate was allowed to pass through the extractor for 61/2 hours. The mixture was cooled and allowed to stand for 16 hours at which point the mixture was warmed to about 40° C., 19 g of sodium carbonate was added, and the solution was stirred for 21/2 hours. The mixture was filtered and vacuum stripped of solvent. The solid residue was extracted with chloroform. Diethyl ether was added to the extract and a polymeric mass precipitated which was discarded. The remaining extract was stripped of solvent to yield 264.2 parts of crude MAGME which was confirmed by chemical analysis.

1. customTo a three-necked flask equipped with a stirrer
2. additionan extractor filled with a molecular sieve drying agent
3. temperatureThe mixture was heated
4. temperatureto reflux
5. custom2 hours
6. temperatureThe mixture was cooled
7. filtrationThe mixture was filtered
8. extractionThe solid residue was extracted with chloroform
9. additionDiethyl ether was added to the
10. extractionextract
11. customa polymeric mass precipitated which
12. extractionThe remaining extract

ORD-Eintrag

ord-c40a641117464e5dbf570addccf5f8fa

Quelldatensatz

uspto-grants-1987_04

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US04656308