Unlock instant, AI-driven research and patent intelligence for your innovation.

The preparation method of amide compound

A technology of amide compounds and compounds, applied in the field of preparation of amide compounds, can solve the problems of harsh reaction conditions, low production efficiency, long reaction time, etc., achieve mild reaction conditions, high production efficiency, and reduce the formation of by-products Effect

Active Publication Date: 2020-08-28
LIANHE CHEM TECH TAIZHOU
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the defects of poor safety, harsh reaction conditions, long reaction time and low production efficiency in the preparation process of amide compounds in the prior art, and to provide a kind of compound with good safety, mild reaction conditions and production efficiency. Preparation method of amides compound with high efficiency and easy operation

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • The preparation method of amide compound
  • The preparation method of amide compound
  • The preparation method of amide compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0064] The reaction formula is as follows:

[0065]

[0066] Preparation of raw materials: Weigh 10.7g of compound I-1, make it into a tetrahydrofuran solution containing 12wt% of compound I-1, and put it in the raw material tank 1; weigh 34mL of 20% n-butyllithium cyclohexane solution, and put it in the raw material tank 2: Weigh 13.4 g of dimethyl carbonate, make it into a tetrahydrofuran solution containing 50 wt% of compound II-1, and put it in the raw material tank 3.

[0067] use figure 1 The process flow diagram, wherein the pipe diameter of the tubular reactor is 10mm, and the reaction pressure is 1.0MPa, according to the following steps: the tetrahydrofuran solution containing compound I-1 in the raw material tank 1 enters the first reaction through the metering pump 1 Zone, the n-butyllithium cyclohexane solution in the raw material tank 2 enters the first reaction zone through the metering pump 2; each metering pump 1 and metering pump 2 are set to control the t...

Embodiment 2

[0070] The reaction formula is:

[0071]

[0072] Preparation of raw materials: weigh 16.9g of compound I-2, make it into a 1,4-dioxane solution containing 11wt% of compound I-2, and put it in the raw material tank 1; weigh 20% n-butyllithium cyclohexane 40 mL of the solution was placed in the raw material tank 2; 18.0 g of diethyl carbonate was weighed to prepare a 1,4-dioxane solution containing 35 wt% of compound II-2, and the solution was placed in the raw material tank 3.

[0073] use figure 1 The process flow diagram, wherein the pipe diameter of the tubular reactor is 10mm, and the reaction pressure is 1.0MPa, according to the following steps: the 1,4-dioxane solution containing compound I-2 in the raw material tank 1 is passed through Metering pump 1 enters the first reaction zone, and the n-butyllithium cyclohexane solution in the raw material tank 2 enters the first reaction zone through the metering pump 2; each metering pump 1 and metering pump 2 are set to con...

Embodiment 3

[0076] The reaction formula is:

[0077]

[0078] Preparation of raw materials: Weigh 12.1g of compound I-3, make it into a methyl tert-butyl ether solution containing 16wt% of compound I-3, and put it in the raw material tank 1; weigh 35mL of 20% n-butyllithium cyclohexane solution , put it in the raw material tank 2; weigh 26.4g of dibenzyl carbonate, make it into a methyl tert-butyl ether solution containing 36wt% compound II-3, and put it in the raw material tank 3.

[0079] use figure 1 The process flow diagram, wherein the tube diameter of the tubular reactor is 10mm, and the reaction pressure is 1.0MPa, according to the following steps: the methyl tert-butyl ether solution containing compound I-3 in the raw material tank 1 is passed through the metering pump 1 enters the first reaction zone, and the n-butyllithium cyclohexane solution in the raw material tank 2 enters the first reaction zone by metering pump 2; each metering pump 1 and metering pump 2 are set to con...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

PropertyMeasurementUnit
wavelengthaaaaaaaaaa
Login to View More

Abstract

The invention discloses a preparation method of an amide compound. The preparation method comprises the following steps: enabling a solution A containing a compound I to react with a solution B containing n-butyllithium at -80 to 10 DEG C, and then enabling a reaction solution to react with a solution C containing a compound II at -80 to 10 DEG C, wherein the concentration of the compound I in the solution A is 5 to 40 percent by weight, the concentration of the compound II in the solution C is 5 to 50 percent by weight, flow rates of the solution A and the solution C are respectively 0.1 to 25 L / s and 0.1 to 1.5 L / s, n is an integer of 0 to 5, and R1 is separately C1 to C6 alkyl, C1 to C6 alkoxy or substituted or un-substituted C6 to C10 aryl; R2 is hydrogen, C1 to C6 alkyl, or substituted or non-substituted phenyl, and a substituting group substituting the phenyl is C1 to C6 alkyl or C1 to C6 alkoxy; and R3 is C1 to C6 alkyl or one or more phenyl-substituted methyl.

Description

technical field [0001] The invention relates to a preparation method of amide compounds. Background technique [0002] In organic synthesis, amides are a class of widely used compounds (J.Biotechol.2016,235,32; Curr.Pharma.Des.2016,22,5029; Org.Biomol.Chem.2016,14,10134; Eur . J. Med. Chem. 2015, 91, 15). [0003] In the synthesis of amide compounds, the acylation of amine compounds is the most direct and effective method to obtain such compounds (Org.ProcessRes.Dev.2016,20,140; Photochem.Rev.2016,15,729; Mol.Bio . Syst. 2015, 11, 338; Sci. Synth. Biocatal. Org. Synth. 2015, 1, 329). [0004] In the acylation reaction of amine compounds, the reaction of n-butyllithium as an added base has the significant advantages of short time, high efficiency and good yield (Chem.Rev.2016,116,12029); however, due to the Lithium has high reactivity, and the reaction system it participates in will quickly release a large amount of heat, resulting in an uncontrollable reaction. Therefore,...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
Patent Type & Authority Patents(China)
IPC IPC(8): C07C269/04C07C271/28
CPCC07C269/04C07C271/28
Inventor 潘强彪邹本立聂良邓陈林渺
Owner LIANHE CHEM TECH TAIZHOU