Sodium Hydroxide → HCID 14459257, compound

Participants

Reaction Steps

1.54 ml (14 mmol) of N,N-dimethylaminoacrolein in 5.3 ml of acetonitrile are added dropwise at 0°-5° C. in the course of 10 minutes under a nitrogen atmosphere to 1.37 ml (15 mmol) of phosphorus oxychloride in 8.5 ml of acetonitrile. After 10 minutes, a solution of 1.3 g (5 mmol) of the compound from Example 4 in 10 ml of acetonitrile is added and the mixture is heated overnight to boiling. 3.7 g of sodium hydroxide in 50 ml of water/50 ml of toluene are added at 10° C., the aqueous phase is washed again with toluene, the organic phases are dried and 0.85 g is obtained after crystallization from ether.

Provenance & Evidence