Patent classifications
C07C45/30
Method for producing oxidation reaction product of hydrocarbon or derivative thereof
The present invention is intended to provide a method that can produce an oxidation reaction product of a hydrocarbon or a derivative thereof in an aqueous phase using a hydrocarbon or a derivative thereof as a raw material. In order to achieve the above object, the method for producing an oxidation reaction product of a hydrocarbon or a derivative thereof of the present invention includes the step of: irradiating a reaction system with light in a presence of a raw material and a halogen oxide radical to react, wherein the raw material is a hydrocarbon or a derivative thereof, the reaction system is a reaction system containing an aqueous phase, the aqueous phase contains the raw material and the halogen oxide radical, and in the reaction step, the raw material is oxidized to produce an oxidation reaction product of the raw material.
Method of preparing 8-methyldecanal
The present invention discloses a novel method of preparing 8-methyldecanal, a flavor and fragrance material. Specifically, starting from cheap and readily available material 6-chloro-1-hexanol, first, the hydroxyl group was protected with dihydropyran catalyzed by para-toluene sulfonic acid to produce 6-chloro-hexyl tetrahydropyran ether. Then 6-chloro-hexyl tetrahydropyran ether reacted with magnesium turnings to form a Grignard reagent and reacted with 1-bromo-2-methyl-butane under the catalysis of cuprous bromide to give the intermediate 8-methyl-sunny tetrahydropyran ether. Without purification, crude 8-methyl-sunny tetrahydropyran ether was treated under acidic conditions to remove the protecting group to generate 8-methyl-1-decyl alcohol. Finally, 8-methyl decanal was obtained after oxidation with 2, 2, 6, 6-tetramethylpiperidinyloxy. The novel method of preparing 8-methyldecanal disclosed in the present invention utilizes common raw materials with low costs, the reaction conditions are mild, and yield is high. It is suitable for large-scale production.
Method of preparing 8-methyldecanal
The present invention discloses a novel method of preparing 8-methyldecanal, a flavor and fragrance material. Specifically, starting from cheap and readily available material 6-chloro-1-hexanol, first, the hydroxyl group was protected with dihydropyran catalyzed by para-toluene sulfonic acid to produce 6-chloro-hexyl tetrahydropyran ether. Then 6-chloro-hexyl tetrahydropyran ether reacted with magnesium turnings to form a Grignard reagent and reacted with 1-bromo-2-methyl-butane under the catalysis of cuprous bromide to give the intermediate 8-methyl-sunny tetrahydropyran ether. Without purification, crude 8-methyl-sunny tetrahydropyran ether was treated under acidic conditions to remove the protecting group to generate 8-methyl-1-decyl alcohol. Finally, 8-methyl decanal was obtained after oxidation with 2, 2, 6, 6-tetramethylpiperidinyloxy. The novel method of preparing 8-methyldecanal disclosed in the present invention utilizes common raw materials with low costs, the reaction conditions are mild, and yield is high. It is suitable for large-scale production.
Process for the preparation of treprostinil
Treprostinil is a synthetic prostacyclin derivative with thrombocyte aggregation inhibitory and vasodilatory activity. Treprostinil can be administered in subcutaneous, intravenous, inhalable, or oral forms. Disclosed is a method for the preparation of treprostinil of formula I and its amorphous form, anhydrate form, monohydrate form, and polyhydrate form salts with bases. In the disclosed method, the chiral center in the 3-hydroxyoctyl substituent is formed at the end of the synthesis, so that the method is robust and well scalable. Also disclosed are treprostinil intermediates and the preparation of the intermediates. ##STR00001##
Process for the preparation of treprostinil
Treprostinil is a synthetic prostacyclin derivative with thrombocyte aggregation inhibitory and vasodilatory activity. Treprostinil can be administered in subcutaneous, intravenous, inhalable, or oral forms. Disclosed is a method for the preparation of treprostinil of formula I and its amorphous form, anhydrate form, monohydrate form, and polyhydrate form salts with bases. In the disclosed method, the chiral center in the 3-hydroxyoctyl substituent is formed at the end of the synthesis, so that the method is robust and well scalable. Also disclosed are treprostinil intermediates and the preparation of the intermediates. ##STR00001##
Process for the preparation of treprostinil
Treprostinil is a synthetic prostacyclin derivative with thrombocyte aggregation inhibitory and vasodilatory activity. Treprostinil can be administered in subcutaneous, intravenous, inhalable, or oral forms. Disclosed is a method for the preparation of treprostinil of formula I and its amorphous form, anhydrate form, monohydrate form, and polyhydrate form salts with bases. In the disclosed method, the chiral center in the 3-hydroxyoctyl substituent is formed at the end of the synthesis, so that the method is robust and well scalable. Also disclosed are treprostinil intermediates and the preparation of the intermediates. ##STR00001##
METAL ORGANIC INTERACTIONS AT HYDROTHERMAL CONDITIONS
Oxidizing a first aromatic compound in the presence of a metal salt to yield a second aromatic compound includes combining the first aromatic compound, the metal salt, and water to yield an aqueous mixture, and heating the aqueous mixture at a temperature exceeding 200° C. to yield a reaction product that includes the second aromatic compound.
METAL ORGANIC INTERACTIONS AT HYDROTHERMAL CONDITIONS
Oxidizing a first aromatic compound in the presence of a metal salt to yield a second aromatic compound includes combining the first aromatic compound, the metal salt, and water to yield an aqueous mixture, and heating the aqueous mixture at a temperature exceeding 200° C. to yield a reaction product that includes the second aromatic compound.
RIPENING OF 1,4-BIS (4-PHENOXYBENZOYL)BENZENE
A method for manufacturing 1,4-bis(4-phenoxybenzoyl)benzene, including: reacting terephthaloyl chloride with diphenyl ether in a reaction solvent and in the presence of a Lewis acid, so as to obtain a product mixture comprising a 1,4-bis(4-phenoxybenzoyl)benzene-Lewis acid complex; putting the product mixture in contact with a protic solvent, so as to obtain a first phase containing the Lewis acid and a second phase containing 1,4-bis(4-phenoxybenzoyl)benzene; heating at least the second phase up to a maximum temperature, followed by cooling the second phase down to a separation temperature; subjecting at least the second phase to a solid/liquid separation step at the separation temperature, so as to recover solid 1,4-bis(4-phenoxybenzoyl)benzene.
Ripening of 1,4-bis (4-phenoxybenzoyl)benzene
A method for manufacturing 1,4-bis(4-phenoxybenzoyl)benzene, including: reacting terephthaloyl chloride with diphenyl ether in a reaction solvent and in the presence of a Lewis acid, so as to obtain a product mixture including a 1,4-bis(4-phenoxybenzoyl)benzene-Lewis acid complex; contacting the product mixture with a protic solvent, so as to obtain a first phase containing the Lewis acid and a second phase containing 1,4-bis(4-phenoxybenzoyl)benzene; heating at least the second phase up to a maximum temperature, followed by cooling the second phase down to a separation temperature; subjecting at least the second phase to a solid/liquid separation step at the separation temperature, so as to recover solid 1,4-bis(4-phenoxybenzoyl)benzene.