Production method for 1-amino cyclopropane carboxylic acid nonhydrate
A technology of aminocyclopropane and hydrate, which is applied in the production field of 1-aminocyclopropanecarboxylic acid non-hydrate, can solve problems such as being unsuitable for industrial production, and achieve the effect of good yield
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Embodiment 1
[0064] To 1-aminocyclopropanecarboxylate hydrochloride (purity 98.7%, 2 g) were added water (2.7 g) and 2-methylpropan-1-ol (4.6 g). Triethylamine (1.5 g) was added thereto to adjust the pH to 6.0, the obtained slurry was cooled to 20°C, and the precipitated crystals were collected by filtration. The obtained crystals were washed with 2-methylpropan-1-ol (10.6 g) to obtain 0.5 hydrate of 1-aminocyclopropanecarboxylic acid.
Embodiment 2
[0066] To a mixture of 1-aminocyclopropanecarboxylate hydrochloride (84.7% purity, 2 g) and 10% hydrochloric acid (4.0 g) was added 2-propanol (5.5 g). To the obtained solution was added triethylamine (2.7 g) to adjust the pH to 5.6, the obtained slurry was cooled to 15°C, and the precipitated crystals were collected by filtration. The obtained wet crystals were washed with 2-propanol (1.7 g) to give 0.5 hydrate of 1-aminocyclopropanecarboxylic acid.
Embodiment 3
[0068] To a mixture of 1-aminocyclopropanecarboxylate hydrochloride (purity: 84.7%, 10 g) and 10% hydrochloric acid (4.0 g) was added 1-butanol (16.8 g). To the obtained solution was added triethylamine (13.2 g) to adjust the pH to 5.6, the obtained slurry was cooled to 16°C, and the precipitated crystals were collected by filtration. The obtained wet crystals were washed with 1-butanol (8.3g), and dried at 50°C under reduced pressure for 3h to obtain 1-aminocyclopropanecarboxylic acid 0.5 hydrate (5.83g, content: 92.0% (yield 86.2%) , water content: 8.0%).
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