* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
2 Preparation Example 2 prilocaine base crude implementation
300ml of acetone was added N- (2- methylphenyl) -2-chloropropionyl amide (Formula ) 35.0g stirred for 15min, stirring was added n-propylamine 10.9g 15min, granular potassium carbonate was added 54.80g.It was heated to reflux for 8-10 hours the reaction start timing.Completion of the reaction, cooling to 5 The oily filtrate was distilled spin dry solvent.Concentrated residue with n-heptane 500ml dissolved, purified water 300ml were washed three times to completely wash out the inorganic salt, the organic layer was evaporated under reduced pressure spin drying solvent to give prilocaine base crude 37.98g, HPLC normalization method purity 98.6%, molar yield about 96%.3 prilocaine base (Formula ) purified in Example35.00 g crude prilocaine base, adding n-heptane (150ml) and ethanol (25ml) consisting of a mixed solvent, stirred and heated to 40 clear solution.After filtration precision filter, down to -15.0 crystallized timing insulation crystallization for 10 hours.Filtration at 20 ~ 25 -0.08Mpa dried under vacuum to dryness to give a pharmaceutical grade prilocaine base 31.1g.Normalization HPLC purity of 99.9% molar yield of 90%.
Chemistry
Pharmaceutical Intermediates
Inhibitors/Agonists
Material Science
For Research Only
110K+ Compounds
Competitive Price
1-2 Day Shipping
