Musk 207 synthesis method
A technology for synthesizing musk and chlorination reaction, applied in the chemical field, can solve the problems of strong corrosiveness, high reaction temperature, and poor drug safety.
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Embodiment 1
[0016] tert-butanol 600ml
[0017] Hydrochloric acid 3000ml
[0018] Aluminum oxide 17g
[0019] m-xylene 800g
[0020] Yihan Reagent 800g
[0021] Acetic acid 160g
[0022] Concentrated nitric acid 240g
[0023] According to the volume ratio, 600ml of tert-butanol and 3000ml of hydrochloric acid were used for chlorination reaction. The chlorination reaction temperature was 5°C, the reaction time was 6hr, and 510g of tert-butyl chloride was isolated. Add 510g of tert-butyl chloride dropwise to the mixture of 17g of aluminum trioxide and 800g of m-xylene, and finish adding in 1.5 hours. The reaction temperature is 1°C, and the temperature is naturally raised for 2 hours. It is ice-thawed, washed with water, alkali, and saturated brine. After reaching neutrality, 450 g of intermediates were produced by distillation and purification. Put 450g of intermediate and 600g of ethanol reagent into the reaction medium, add dropwise 600g of mixed acid (composed of 160g of acetic aci...
Embodiment 2
[0025] tert-butanol 500ml
[0026] Hydrochloric acid 2000ml
[0027] Aluminum oxide 10g
[0028] Yihan Reagent 500g
[0029] Acetic acid 120g
[0030] Concentrated nitric acid 200g
[0031] According to the volume ratio, 500ml of tert-butanol and 2000ml of hydrochloric acid were used for chlorination reaction, the chlorination reaction temperature was 10°C, the reaction time was 6hr, and 420g of tert-butyl chloride was isolated. Add 420g of tert-butyl chloride dropwise to the mixture of 10g of aluminum oxide and 500g of m-xylene, and complete the addition in 1.3 hours. The reaction temperature is 10°C, and the temperature is naturally raised for 2 hours. It is ice-thawed, washed with water, alkali, and saturated brine. After reaching neutrality, 362g of intermediate was produced by distillation and purification. Put 362g of intermediate and 370g of ethanol reagent into the reaction medium, add dropwise 450g of mixed acid (composed of 120g of acetic acid, 200g of concentra...
Embodiment 3
[0033] tert-butanol 500ml
[0034] Hydrochloric acid 1000ml
[0035] Aluminum oxide 10g
[0036] Yihan Reagent 510g
[0037] Acetic acid 160g
[0038] Concentrated nitric acid 180g
[0039] According to the volume ratio, 500ml of tert-butanol and 1000ml of hydrochloric acid were used for chlorination reaction. The chlorination reaction temperature was 30°C, the reaction time was 6hr, and 320g of tert-butyl chloride was isolated. Add 320g of tert-butyl chloride dropwise to the mixture of 10g of aluminum oxide and 400g of m-xylene, and complete the addition in 1.3 hours. The reaction temperature is 20°C, and the temperature is naturally raised for 2 hours. It is ice-thawed and washed with water, alkali, and saturated brine. After reaching neutrality, 260 g of intermediates were produced by distillation and purification. Put 260g of the intermediate and 350g of the ethanol reagent into the reaction medium, add dropwise 500g of mixed acid (composed of 160g of acetic acid, 180...
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