14205-39-1

105-45-3

14205-39-1

The general procedure for the synthesis of methyl 3-aminocrotonate from methyl acetoacetate was as follows: 25 kg of methyl acetoacetate and 20 kg of methanol were pumped into an ammoniation reactor. The temperature of the reaction system was controlled in the range of 0-10°C using an ice-water bath with continuous stirring, and the ammonia was slowly introduced until white crystals were precipitated, and then the introduction of ammonia was stopped. The reaction mixture was allowed to stand under refrigeration overnight and then centrifuged to collect the white crystals. The resulting white crystals were transferred to an ammonia refining kettle and purified by adding 15 kg of methanol, heating the mixture until complete dissolution, followed by cryocrystallization. The mixture was centrifuged again and filtered to collect the filter cake. The filter cake was placed in a hot air circulating oven and dried at 50-60 °C for 8 hours to give 18.6 kg of methyl 3-aminocrotonate. The product needs to be stored at 0 to -10°C for 20 to 24 hours. The yield of this process was 21 kg with a weight yield range of 74.4-84.0% and a molar yield range of 75.0-85.0%.