C07C245/16

AUTOMATED DIAZOMETHANE GENERATOR, REACTOR AND SOLID PHASE QUENCHER

A process for producing diazomethane of Formula 1 (CH.sub.2N.sub.2), with an automated apparatus is described. A stock solution of N-methyl-N-nitroso amine in an organic solvent is continuously flown and mixed with an aqueous inorganic base at a T-mixer to form a mixture. Then it is passed through a capillary micro reactor at a temperature in a range of 20 to 30° C. to form diazomethane. The mixture is separated into an aqueous layer and an organic layer using a continuous flow micro-separator. The organic layer has 0.1-0.4 M diazomethane. The organic layer is reacted with a carboxylic acid, phenol, an alkyne, an anhydride, a carboxyl metal organic framework (MOF), or MOF coated cotton to form a corresponding ester, a pyrazole, an ether, a diazo ketone, a stable carboxyl MOF or a stable MOF coated cotton fiber.

AUTOMATED DIAZOMETHANE GENERATOR, REACTOR AND SOLID PHASE QUENCHER

A process for producing diazomethane of Formula 1 (CH.sub.2N.sub.2), with an automated apparatus is described. A stock solution of N-methyl-N-nitroso amine in an organic solvent is continuously flown and mixed with an aqueous inorganic base at a T-mixer to form a mixture. Then it is passed through a capillary micro reactor at a temperature in a range of 20 to 30° C. to form diazomethane. The mixture is separated into an aqueous layer and an organic layer using a continuous flow micro-separator. The organic layer has 0.1-0.4 M diazomethane. The organic layer is reacted with a carboxylic acid, phenol, an alkyne, an anhydride, a carboxyl metal organic framework (MOF), or MOF coated cotton to form a corresponding ester, a pyrazole, an ether, a diazo ketone, a stable carboxyl MOF or a stable MOF coated cotton fiber.

Process for the preparation of cyclopropane compounds using diazo-compounds
11780803 · 2023-10-10 · ·

A process for the continuous production of a reaction product of a diazo-compound and a substrate in a multi-stage flow reactor is disclosed.

Process for the preparation of cyclopropane compounds using diazo-compounds
11780803 · 2023-10-10 · ·

A process for the continuous production of a reaction product of a diazo-compound and a substrate in a multi-stage flow reactor is disclosed.

Preparation process of diazomethane
20220242818 · 2022-08-04 ·

Provided is a preparation process of diazomethane. The preparation process includes: step S1, taking N-methylurea as a raw material to continuously prepare, in a continuous reactor, a first product system containing N-methyl-N-nitrosourea; step S2, performing continuous extraction and continuous back-extraction on the first product system to obtain an N-methyl-N-nitrosourea solution; step S3, enabling the N-methyl-N-nitrosourea solution to continuously react with an alkaline solution in a continuous reactor to obtain a second product system containing the diazomethane; and step S4, performing continuously liquid separation, water freezing and removal on the second product system, to obtain the diazomethane.

Preparation process of diazomethane
20220242818 · 2022-08-04 ·

Provided is a preparation process of diazomethane. The preparation process includes: step S1, taking N-methylurea as a raw material to continuously prepare, in a continuous reactor, a first product system containing N-methyl-N-nitrosourea; step S2, performing continuous extraction and continuous back-extraction on the first product system to obtain an N-methyl-N-nitrosourea solution; step S3, enabling the N-methyl-N-nitrosourea solution to continuously react with an alkaline solution in a continuous reactor to obtain a second product system containing the diazomethane; and step S4, performing continuously liquid separation, water freezing and removal on the second product system, to obtain the diazomethane.

Method and Device for Continuously Synthesizing Cyclopropane Compounds
20220242805 · 2022-08-04 ·

The present disclosure discloses a method and a device for continuously synthesizing cyclopropane compounds. The method includes the following steps: continuously performing a synthetic reaction of a diazomethane precursor in a first reactor, the reaction product of the first reactor flowing into a separator for stratification, the organic phase obtained by stratification overflowing into a second reactor, continuously consuming the diazomethane precursor in a second reactor to prepare diazomethane and performing an electron-rich monoolefin cyclopropanation reaction in situ so as to obtain the cyclopropane compound. The technical solution of the present disclosure may be applied to achieve automatic control, decrease the transfer of high-risk materials, and prevent the risk of pipeline transfer of diazomethane solution, and effectively improve production safety. Moreover, the present disclosure provides a simple device to save equipment investment, and may safely and quantitatively achieve the production of diazomethane and the cyclopropanation reaction of olefins simultaneously.

PROCESS FOR THE PREPARATION OF CYCLOPROPANE COMPOUNDS USING DIAZO-COMPOUNDS
20210253514 · 2021-08-19 ·

A process for the continuous production of a reaction product of a diazo-compound and a substrate in a multi-stage flow reactor is disclosed.

PROCESS FOR THE PREPARATION OF CYCLOPROPANE COMPOUNDS USING DIAZO-COMPOUNDS
20210253514 · 2021-08-19 ·

A process for the continuous production of a reaction product of a diazo-compound and a substrate in a multi-stage flow reactor is disclosed.

Preparation process of diazomethane

Provided is a preparation process of diazomethane. The preparation process includes: step S1, taking N-methylurea as a raw material to continuously prepare, in a continuous reactor, a first product system containing N-methyl-N-nitrosourea: step S2, performing continuous extraction and continuous back-extraction on the first product system to obtain an N-methyl-N-nitrosourea solution; step S3, enabling the N-methyl-N-nitrosourea solution to continuously react with an alkaline solution in a continuous reactor to obtain a second product system containing the diazomethane; and step S4, performing continuously liquid separation, water freezing and removal on the second product system, to obtain the diazomethane.