Preparation method for purified 3-methyl-2-butenyl acetate
A technology of methyl and acetic acid, applied in chemical instruments and methods, preparation of carboxylate, preparation of organic compounds, etc., can solve problems such as low yield, amine compound treatment of wastewater, and dissatisfaction
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Embodiment 1
[0035] Embodiment 1 (reaction steps)
[0036] Under a nitrogen atmosphere, 140.6g (1.60mol) of 3-methyl-2-buten-1-ol (content: 98% by weight) and 16.2g (0.16mol) of potassium acetate (content: 97% by weight) Mixing is performed and the mixture is heated to 48 to 52°C. 176.85 g (1.68 mol) of acetic anhydride (content: 97% by weight) was added dropwise to the mixture over 5 hours, and then the mixture was continuously stirred at the same temperature for 6 hours. The reaction mixture was analyzed by gas chromatography internal standard method, and the yield of (3-methyl-2-butenyl) acetate was found to be 100% (based on 3-methyl-2-buten-1-ol). The reaction mixture was cooled to 28 to 32°C. After 35.2 g of water was added dropwise thereto within 1 hour, 105.5 g of water was added thereto, and the mixture was continuously stirred at the same temperature for 1 hour. The reaction mixture was left standing and separated to obtain 261.5 g of an organic layer containing (3-methyl-2-bu...
Embodiment 2
[0040] Embodiment 2 (purification step)
[0041] 83.7 g of a 5% aqueous solution of sodium bisulfite was added to the organic layer obtained in Example 1, the mixture was stirred at 20 to 30° C. for 1 hour, and then the mixture was left to stand and separated to obtain an organic layer. 70.3 g of water was added to the organic layer, the mixture was stirred at the same temperature for 30 minutes, and then the mixture was left to stand and separated to obtain an organic layer. The organic layer was cooled to 15 to 25°C, 44.9 g of a 30% potassium carbonate aqueous solution was added dropwise thereto, and then 67.3 g of a 5% sodium bicarbonate aqueous solution was added thereto. The mixture was stirred at the same temperature for 30 minutes, and then the mixture was left to stand and separated to obtain an organic layer. 70.3 g of water was added to the organic layer, the mixture was stirred at the same temperature for 30 minutes, and then, the mixture was left to stand and sepa...
Embodiment 3
[0045] Embodiment 3 (reaction steps)
[0046] Under a nitrogen atmosphere, 552.9 g (6.40 mol) of 3-methyl-2-buten-1-ol (content: 99.7% by weight) and 48.6 g (0.48 mol) of potassium acetate (content: 97% by weight) Mixing is performed and the mixture is heated to 48 to 52°C. 707.3 g (6.72 mol) of acetic anhydride (content: 97% by weight) was added dropwise to the mixture over 5.5 hours, and then the mixture was continuously stirred at the same temperature for 9 hours. The reaction mixture was analyzed by gas chromatography internal standard method, and the yield of (3-methyl-2-butenyl) acetate was found to be 100% (based on 3-methyl-2-buten-1-ol). The reaction mixture was cooled to 28 to 32°C. After 138 g of water was added dropwise thereto within 1 hour, 415 g of water was added thereto, and the mixture was continuously stirred at the same temperature for 1 hour. The reaction mixture was left to stand and separated to obtain 1045.7 g of an organic layer containing (3-methyl...
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