Beta-carotene preparing process
A carotene and Grignard technology, which is applied in the field of preparation of beta-carotene, can solve the problems of difficulty in removing triphenylphosphine oxide, difficulty in reaching production scale, limited source of raw materials, etc., and achieves low cost, convenient operation and simple method. Effect
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Embodiment 1
[0025] A. trans C 6 Preparation of phosphonium salts
[0026] Add C to a 500ml three-neck flask 6 Alcohol ((E)-3-methyl-2-ene-4-yne-1-pentanol) 9.6g, dichloromethane 200ml, add 58% hydrobromic acid 20g dropwise at room temperature, and keep warm for 30 minutes after dropping , 100 ml of water was added, and the dichloromethane layer was separated. Concentrate the dichloromethane layer to 50ml, add ethyl acetate 150ml, PPh 3 28g, reacted at room temperature for 24 hours, filtered and dried to obtain C 6 Phosphonium salt 26g. The mother liquor is concentrated to about 100ml, cooled, and C can be precipitated 6 Phosphonium salt 8g, yield 81%.
[0027] B.C. 22 Preparation of Diyne Polyene Compound (U)
[0028] Add 21g of C into a 1000ml four-neck flask 6 Phosphine salt, 4g C10 aldehyde ((2E,4E,6E)-2,7-dimethyl-2,4,6-octatrienedialdehyde), 250ml methanol, control the reaction temperature at about 10°C, stir and drop 10 70ml of methanol solution of potassium tert-butoxide....
Embodiment 2
[0034] A, prepare trans C in the same way as in Example 1 6 Phosphonate and C 22 Diacetylenic polyene compound
[0035] B, the preparation of double dehydrobeta-carotene (W)
[0036] Add 300ml of diethyl ether, 2.6g of Mg, 2g of bromoethane and 0.1g of iodine into a 1000ml flask, heat it to initiate, then control the reaction temperature at 30-35°C, add the remaining 12g of bromoethane dropwise, finish the drop, and keep the temperature for reaction until Mg disappears completely. Then add 14.4g C in batches to the above reaction solution 22 Diyne polyene compound (U), heat preservation reaction until a uniform viscous solution is formed. Raise the temperature to 50°C, add dropwise a 200ml diethyl ether solution containing 24g of 2,2,6-trimethylcyclohexanone (A). % dilute sulfuric acid 100ml, 3 x 400ml CHCl 3 Extraction, CHCl 3 The layer was washed with 3×200ml water, and the CHCl was removed under reduced pressure 3 , 22.8 g of double dehydroβ-carotene was obtained, a...
Embodiment 3
[0040] A, prepare trans C in the same way as in Example 1 6 Phosphonate and C 22 Diacetylenic polyene compound
[0041] B, the preparation of double dehydrobeta-carotene (W)
[0042] Add 300ml of diethyl ether, 2.6g of Mg, 2g of bromoethane and 0.1g of iodine into a 1000ml flask, heat it to initiate, then control the reaction temperature at 30-35°C, add the remaining 12g of bromoethane dropwise, finish the drop, and keep the temperature for reaction until Mg disappears completely. Then add 14.4g C in batches to the above reaction solution 22 Diyne polyene compound (U), heat preservation reaction until a uniform viscous solution is formed. Raise the temperature to 50°C, add dropwise a 200ml ether solution containing 49g of 2,2,6-trimethylcyclohexanone (A). % dilute sulfuric acid 100ml, 3 x 400ml CHCl 3 Extraction, CHCl 3 The layer was washed with 3×200ml water, and the CHCl was removed under reduced pressure 3 , 23.6 g of double dehydroβ-carotene was obtained, with a yi...
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