2-Mercaptoethanol → Butanoic acid, 3-oxo-, 2-mercaptoethyl ester

Temperature

130 °C

In a 300 ml. round bottom flask fitted with a thermometer, mechanical stirrer, Dean Stark trap and reflux condenser was placed 25.0g.(0.32 mole) of 2-mercaptoethanol. This was stirred and heated to 130° C.; 45.4g. (0.32 mole) of 2,2,6-trimethyl-1,3-dioxen-4-one (TKD) was added dropwise at a uniform rate over the period of one hour. Heating was continued for 1/2 hour; acetone distillate was collected in the Dean Stark trap. After distillate collection was completed, the mixture was distilled under vacuum and the portion boiling at 110°-115° C.(at 5 mm. Hg.) was collected to give a colorless liquid of mercaptoethylacetoacetate. The yield was about 90% based on starting material. The product was identified by NMR spectroscopy.

1. customround bottom flask fitted with a thermometer, mechanical stirrer, Dean Stark trap
2. temperaturereflux condenser
3. temperatureHeating
4. distillationacetone distillate was collected in the Dean Stark trap
5. distillationAfter distillate collection
6. distillationthe mixture was distilled under vacuum
7. customthe portion boiling at 110°-115° C.(at 5 mm. Hg.) was collected

ORD record

ord-e08a171b5cee4274b723cba3e8ea35b9

Source dataset

uspto-grants-1990_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04960924