Acetonitrile → HCID 87359877, compound

Participants

Reaction Conditions

Reaction Steps

Acetonitrile (692.5 g) and diketene (46.5 g) were introduced into a 5,000 mL four-necked flask, and the mixture was cooled so that the temperature in the flask was lowered to −5 to 0° C. Diketene and 2-(ethylamino)ethanol were simultaneously added dropwise for 4 hours at a rate of 220 g/h and 233.5 g/h, respectively. During the addition, cooling was suitably conducted to maintain the temperature in the flask at −5 to 0° C. Thereafter, 30 g of 2-(ethylamino)ethanol was added dropwise at a rate of 233.5 g/h. The resultant was heated to room temperature and aged for 12 hours. Then, while the mixture in the flask was heated to a temperature of 40 to 50° C., acetonitrile was removed under reduced pressure, and the resulting mixture was finally kept at a pressure of about 0.001 for 4 hours, to thereby produce about 1,850 g of 2-(N-ethyl-N-(2-acetylacetyl)aminoethanol.

Provenance & Evidence