33 results about "Piperonal" patented technology

The invention relates to an asymmetric synthesis method of (+)-tanshinol, which comprises the following steps: carrying out Knoevenagel condensation on the raw material heliotropin, hydrolyzing for ring opening to obtain beta-(3,4-3,4-methylenedioxyphenyl)pyruvic acid, carrying out key asymmetric reduction reaction to obtain R-beta-(3,4-dibenzyloxyphenyl)-alpha-hydracrylic acid, and finally, deprotecting to obtain the (+)-tanshinol. The method has the advantages of accessible raw material and high optical purity of the product, is simple to operate, and can implement large-scale preparation.

Pest control compositions, blends, and formulations are disclosed. The blends contain, in a synergistic combinations, at least two ingredients such as Lilac Flower Oil, D-Limonene, Thyme Oil, Lime Oil, Black Seed Oil, Wintergreen Oil, Linalool, Tetrahydrolinalool, Vanillin, Isopropyl myristate, Piperonal (aldehyde), Geraniol, Geraniol 60, Triethyl Citrate, and Methyl Salicylate.

The invention discloses a preparation method of tadalafil, starting material D-Tryptophan methyl ester hydrochloride is reacted with oxalyl chloride to obtain an intermediate III, and the final product tadalafil (I) is obtained through cyclization, Grignard reaction, asymmetric reduction, substitution and condensation reaction. The use of national control chemical piperonal is avoided, an intermediate VI can be highly-selectively obtained by the asymmetric reduction, and the method has the advantages of simple postprocessing, short synthesis steps and high product total yield, and is suitable for industrialized production.

The invention relates to a preparation method of piperonal. The specific steps are: mix water, glyoxylic acid and sulfuric acid in proportion, add piperonyl cyclocyclone dropwise at a temperature of 0-5°C, stir at a high speed for 5-8 hours, add After diluting with 80-100ml of water, filter with suction to obtain solid 3,4-dimethoxymandelic acid, and the filtrate is the mother liquor containing dilute sulfuric acid; the mass ratio of water, glyoxylic acid, and sulfuric acid is 1.5-1.7:10- 11:10‑11; take 30%‑70% dilute sulfuric acid mother liquor, add solid 3,4‑dimethoxymandelic acid to it, then add 80 mL of dichloromethane, add 3% dilute nitric acid 18‑1 dropwise at 20°C 20mL, heated, and reacted for 1-3 hours until the reaction was complete; layers were separated, washed, concentrated and distilled under reduced pressure to obtain the product piperonal.

The invention belongs to the field of organic chemical synthesis, and particularly relates to a synthesis method of homopiperony lamine. The synthesis method comprises the following steps: preparing heliotropin by using catechol as a raw material; preparing beta-nitro-3, 4-dioxomethine styrene from heliotropin; and preparing the homopiperony lamine by using the beta-nitro-3, 4-dioxomethylenestyrene. The method for preparing heliotropin by using catechol as the raw material comprises the following two ways: (1) catechol -> 3,4-dihydroxy mandelic acid -> 3, 4-dihydroxy benzaldehyde -> heliotropin; and (2) catechol -> benzodioxole -> heliotropin. The used raw materials are safe, easy to obtain and low in cost; reaction conditions are mild, operation is simple and convenient, chemical yield is high, and intermediate reagents are easy to recover; and the method is suitable for industrial production.

The invention discloses a method for preparing Tadalafil by a one-pot method. The method for preparing the Tadalafil by the one-pot method comprises the steps that D-Tryptophan methyl ester hydrochloride and piperonal are used as starting materials, and a single-configuration high-purity compound I hydrochloride is obtained through a Pictet-Spengler reaction; the compound I hydrochloride is subjected to an acylation reaction with chloroacetyl chloride in an organic base system of an aprotic solvent to obtain a mixed reaction solution; and the mixed reaction solution is directly added to a methylamine solution to undergo an aminolysis cyclization reaction without treatment, and the mixture is subjected to cooling crystallization to obtain the Tadalafil after the reaction. According to the method for preparing the Tadalafil by the one-pot method, the usage amount of the solvent is reduced, the amount of waste liquid discharge is effectively controlled, and environmental protection is facilitated; the production cycle is shortened, and the process efficiency is improved; and the yield is improved, and the cost is reduced. Compared with an existing process route, the method for preparing the Tadalafil by the one-pot method is more environmentally friendly, more efficient and lower in cost, and is more suitable for industrial production.

The invention discloses a preparation method of a phosphodiesterase inhibitor, belonging to the field of medicinal chemistry. The preparation method comprises the following steps: carrying out an esterification reaction on an initial raw material 1 and methanol to prepare an intermediate I, directly carrying out condensation cyclization on the intermediate I and heliotropin to prepare an intermediate II, and carrying out chloracetylation, aminolysis cyclization and refining to prepare a final product, namely a refined tadalafil product. The method improves product yield and quality, greatly shortens a reaction period in a preparation process, reduces operation steps and production cost, and is suitable for industrial mass production.

The invention discloses a preparation method of a medical intermediate 6-amino heliotropin, wherein the method comprises the following steps: S1, adding heliotropin into concentrated nitric acid to react, and pouring into water; S2, extracting with an organic solvent, and collecting an organic phase; S3, adding potassium permanganate into the organic phase, reacting at the temperature of 90-120 DEG C, filtering to remove solids, and collecting filtrate; and S4, adding a palladium-carbon catalyst into the filtrate, reducing at the temperature of 80-100 DEG C in the presence of a mixed gas of hydrogen and inert gas to obtain a crude product, and recrystallizing the crude product. Compared with the prior art, the preparation method has the advantages that the purification step of an intermediate product is omitted; the yield of the final product 6-amino heliotropin is about 40-50%, so that the raw material utilization rate is remarkably improved, the operation efficiency of enterprises isimproved, the time cost and the material cost are saved for the enterprises, and the method has a wide industrial prospect.