Acetic Anhydride → HCID 322651, compound

Temperature

60 °C

A mixture of L-glutamic acid (40 g, 0.272 mole), triethylamine (100 ml), acetic anhydride (100 ml) and 4-(dimethylamino)pyridine (0.25 g) is heated at 60° C. with magnetic stirring overnight. The dark solution is removed of volatile materials by distillation at 85° C. at 10 mm Hg. The residue is mixed with 50 ml of 10 percent HCl and extracted with methylene chloride (2×100 ml). The methylene chloride solution is washed with saturated brine and dried over anhydrous magnesium sulfate. After removal of the drying agent and the solvent, the residue is subjected to vacuum distillation to give 30.5 g (66 percent yield) of the desired product, b.p. (0.1 mm) 90° C.-92° C., which solidified rapidly on standing.

1. customThe dark solution is removed of volatile materials by distillation at 85° C. at 10 mm Hg
2. additionThe residue is mixed with 50 ml of 10 percent HCl
3. extractionextracted with methylene chloride (2×100 ml)
4. washThe methylene chloride solution is washed with saturated brine
5. dry with materialdried over anhydrous magnesium sulfate
6. customAfter removal of the drying agent
7. distillationthe solvent, the residue is subjected to vacuum distillation

ORD record

ord-298c1b23c81142dc870a2a32e19465d2

Source dataset

uspto-grants-1990_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04943640