A kind of preparation method of hepatitis C medicine intermediate
A technology of intermediates and drugs, which is applied in the field of preparation of hepatitis C drug intermediates, can solve the problems of reducing process costs, difficulty in industrialization, and high cost, and achieve the effect of reducing process costs and realizing feasibility
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Embodiment 1
[0033] The 500ml three-necked flask is equipped with a mechanical stirrer, a thermometer, and a condensation reflux tube. At 45°C, add 38.6g of D-di-p-toluyl tartaric acid (D-DTTA) (0.1mol), 200g of ethanol, 20g of water, stir to dissolve, and dropwise add 15.5g of 1-amino-2-vinylcyclopropanyl formic acid Ethyl ester, a solid is produced during the process. Raise the temperature to reflux to dissolve and clarify, then slowly cool down to 20°C, crystallize, filter with suction, and dry to obtain (1R,2S)-1-amino-2-vinylcyclopropane ethyl carboxylate D-di-p-methylbenzene Formyl tartaric acid (D-DTTA) salt is a white solid, the enantiomeric excess (ee) value is 77.5% and the yield is 38.9%.
[0034] The 500ml three-necked flask is equipped with a mechanical stirrer, a thermometer, and a condensation reflux tube. Add 50g of (1R,2S)-1-amino-2-vinylcyclopropane ethyl carboxylate D-di-p-toluyl tartaric acid (D-DTTA) salt prepared in the previous step, 500g of ethanol, 50g of water, ...
Embodiment 2
[0038] The 500ml three-necked flask is equipped with a mechanical stirrer, a thermometer, and a condensation reflux tube. At 40°C, add 38.6g of D-di-p-toluyl tartaric acid (D-DTTA) (0.1mol), 150g of methanol, 20g of water, stir to dissolve, and dropwise add 15.5g of 1-amino-2-vinylcyclopropanyl formic acid Ethyl ester, a solid is produced during the process. Heat up to reflux to dissolve and clarify, then slowly cool down to 25°C, crystallize, filter with suction, and dry to obtain (1R,2S)-1-amino-2-vinylcyclopropanylcarboxylate D-DTTA salt white solid, The enantiomeric excess (ee) value of the sample sent was 80.7%, and the yield was 37.2%.
[0039] The 500ml three-necked flask is equipped with a mechanical stirrer, a thermometer, and a condensation reflux tube. Add 50g of (1R,2S)-1-amino-2-vinylcyclopropane ethyl carboxylate D-di-p-toluyl tartaric acid (D-DTTA) salt prepared in the previous step, 450g methanol, 60g water, and heat up Dissolve and clarify at reflux, then s...
Embodiment 3
[0042] The 500ml three-necked flask is equipped with a mechanical stirrer, a thermometer, and a condensation reflux tube. At 30°C, add 38.6g D-di-p-toluyl tartaric acid (D-DTTA) (0.1mol), 250g isopropanol, 40g water, stir to dissolve, add dropwise 15.5g 1-amino-2-vinylcyclopropane Ethyl formate, solids are generated during the process. Raise the temperature to reflux to dissolve and clarify, then slowly cool down to 15°C, crystallize, filter with suction, and dry to obtain (1R,2S)-1-amino-2-vinylcyclopropane ethyl carboxylate D-di-p-methylbenzene Formyl tartaric acid (D-DTTA) salt is a white solid, the enantiomeric excess (ee) value is 77.1% and the yield is 40.4%.
[0043] The 500ml three-necked flask is equipped with a mechanical stirrer, a thermometer, and a condensation reflux tube. Add 50g of (1R,2S)-1-amino-2-vinylcyclopropane ethyl carboxylate D-di-p-methylbenzoyl tartaric acid (D-DTTA) salt prepared in the previous step, 600g of isopropanol, 100g of water , heat up ...
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