(r) The synthetic method of -5-methylpyrrolidone-2-one
A technology of methyl pyrrolidone and a synthesis method, applied in the directions of organic chemistry, organic chemistry, etc., can solve the problems of expensive raw materials, high production cost, weak universality and the like, and achieves high atom utilization, easy purification, The effect of low raw material prices
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Embodiment 1
[0033] Example 1: In a 1L three-necked flask, add 500mL of dichloromethane, cool down in an ice bath by about 5 degrees, feed 80g of methyl levulinate, 17g of (S)-Me-CBS, pass nitrogen flow, and dropwise add borane dimethyl 56.04g of thioether, stirred for 0.5h after dropping, heated up to 30°C for 3h, and HPLC detected the end of the reaction. Methanol was added dropwise, and the reaction was quenched with hydrochloric acid. After the treatment, 69.8 g of methyl (R)-4-hydroxyvaleric acid was obtained, >99% ee, and the yield was 85.8%.
[0034] Put 50g of (R)-methyl 4-hydroxypentanoate into a 2L autoclave, add 400g of ammonia water, 400g of methanol, and 5g of Raney nickel, close the lid, replace the nitrogen, and let the hydrogen flow to 4 kg. The temperature was raised to 90°C, and the reaction was completed in 6 hours. The catalyst was filtered, extracted with water and EA, and 48 g of (R)-4-aminovaleric acid methyl ester was obtained after treatment, with a yield of 96.8%...
Embodiment 2
[0036] Example 2: In a 1L three-necked flask, add 500mL of acetonitrile, cool down in an ice bath by about 5 degrees, feed 80g of methyl levulinate, 17g of (S)-Me-CBS, pass nitrogen flow, and add borane dimethyl sulfide dropwise 56.04g, stirred for 0.5h after dropping, heated up to 30°C for 3h, and HPLC detected the end of the reaction. Methanol was added dropwise, and the reaction was quenched with hydrochloric acid. After the treatment, 70.5 g of (R)-4-hydroxyvaleric acid methyl ester was obtained, >99% ee, and the yield was 86.6%.
[0037] Put 50g of (R)-methyl 4-hydroxypentanoate into a 2L autoclave, add 400g of ammonia water, 400g of methanol, and 5g of Raney nickel, close the lid, replace the nitrogen, and let the hydrogen flow to 4 kg. The temperature was raised to 90°C, and the reaction was completed in 6 hours. The catalyst was filtered, extracted with water and EA, and 47 g (R)-4-aminovaleric acid methyl ester was obtained after treatment, with a yield of 94.8%.
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Embodiment 3
[0039]Example 3: In a 1L three-necked flask, add 500mL of dimethylformamide, cool down in an ice bath by about 5°C, feed 80g of methyl levulinate, 17g of (S)-Me-CBS, pass nitrogen flow, and add borane dropwise 56.04g of dimethyl sulfide, stirred for 0.5h after dropping, heated up to 30°C for 3h, and HPLC detected the end of the reaction. Methanol was added dropwise, and the reaction was quenched with hydrochloric acid. After the treatment, 70 g of (R)-methyl 4-hydroxyvalerate was obtained, >99% ee, and the yield was 86%.
[0040] Put 50 g of (R)-methyl 4-hydroxypentanoate into a 2L autoclave, add 400 g of ammonia water, 400 g of methanol, and 5 g of Raney nickel, cover the lid, replace the nitrogen, and pass the hydrogen to 4 kg. The temperature was raised to 90°C, and the reaction was completed in 6 hours. The catalyst was filtered, extracted with water and EA, and 49 g of (R)-4-aminovaleric acid methyl ester was obtained after treatment, with a yield of 98.8%.
[0041] Put...
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