N-(2-Cyano-3-hydroxy-2-propenyl)formamide Monosodium Salt synthesis

Yield:106030-08-4 93.8%

Reaction Conditions:

with sodium ethanolate at -10 - 70; under 37503.8 - 45004.5 Torr; for 10 h;Autoclave;Temperature;Pressure;Reagent/catalyst;

Steps:

2 Embodiment 1

Add 284 g of ethyl formate to a 500 mL three-neck bottle.At a certain temperature (see Table 1 for specific temperature selection), slowly add 35g of solid sodium ethoxide at a rate of 1.2g/min and raise the temperature to 10 °C.Then add 30 g of β-aminopropionitrile at a rate of 1.0 g/min.The above reaction solution was poured into a 500 mL autoclave, and stirring was started.Heating to raise the temperature to 65-70 ° C,The pressure range is 5.0-6.0MPa, and it will naturally drop to 20°C after 10h of heat preservation.After suction filtration, the filter cake was washed twice with 25 g of ethyl formate, and the filter cake was dried at 50 ° C.getΑ-formyl-β-formylaminopropionitrileYellowish solid sodium salt 65.8g,The content is 90.4%,The yield was 93.8%.

References:

CN108484439,2018,A Location in patent:Paragraph 0013-0014; 0016; 0018; 0020; 0022; 0024; 0026-0027