Preparation method of acetamide compound

A compound, acetamide technology, applied in the field of preparation of acetamide compounds, can solve problems such as the effect of equipment corrosion

Active Publication Date: 2021-05-18
ZHEJIANG SCI-TECH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the reaction process, HI is often used as a co-catalyst, which has a serious corrosion effect on the equipment

Method used

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  • Preparation method of acetamide compound
  • Preparation method of acetamide compound
  • Preparation method of acetamide compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1～15

[0036] Add dirhodium tetracarbonyl dichloride, 1,3-bis(diphenylphosphine)propane (DPPP), tungsten carbonyl, sodium phosphate, sodium iodide, water, Nitro compound (II) and dimethyl carbonate (III), mixed and stirred evenly, reacted according to the reaction conditions in Table 2, after the reaction was completed, filtered, silica gel mixed sample, and purified by column chromatography to obtain the corresponding acetamide compound (Ⅰ ), the reaction process is shown in the following formula:

[0037]

[0038] The raw material addition of table 1 embodiment 1~15

[0039]

[0040] Table 2

[0041]

[0042] In Table 1 and Table 2, T is the reaction temperature, t is the reaction time, Et is ethyl, Ph is phenyl, CF 3 is trifluoromethyl, Me is methyl, SMe is methylthio, OMe is methoxy, and t-Bu is tert-butyl.

[0043] The structural confirmation data of the compounds prepared in Examples 1-5:

[0044] The nuclear magnetic resonance (NMR) of the acetamide compound (I-1)...

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PUM

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Abstract

The invention discloses a preparation method of an acetamide compound, the preparation method comprises the following steps: reacting tetracarbonyl dichloride rhodium, 1, 3-bis (diphenylphosphine) propane, tungsten carbonyl, sodium phosphate, sodium iodide, water, a nitro compound and dimethyl carbonate at 120 DEG C for 24 hours, and after the reaction is completed, performing post-treatment to obtain the acetamide compound. According to the preparation method, dimethyl carbonate serves as a C1 source and also serves as a green solvent, operation is easy, reaction starting raw materials are low in price and easy to obtain, the tolerance range of substrate functional groups is wide, and reaction efficiency is high. Various acetamide compounds can be synthesized according to actual needs, so that the practicability of the method is widened while the operation is convenient.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a preparation method of acetamide compound. Background technique [0002] Dimethyl carbonate is a class of low-toxic, biodegradable compounds that can be converted from carbon dioxide in the atmosphere and is often used as a green solvent in organic synthesis (Chem. Rev. 2010, 110, 4554-4581), Has a very broad development prospects. At the same time, as an important intermediate in organic synthesis, dimethyl carbonate has a wide range of applications in industry and fine chemistry. Under different reaction conditions, dimethyl carbonate can act as both a methoxycarbonylating reagent and a methylating reagent to react with various nucleophiles (Green Chem. 2018, 20, 28-85). Conventional methylation reagents such as diazomethane, dimethyl sulfate, and methyl iodide mostly have the disadvantages of being explosive, toxic / corrosive, and expensive. Furthermore, stoichiometric amou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C231/10C07C233/25C07C233/15C07C233/14C07D317/66
CPCC07C231/10C07D317/66C07C2601/14C07C233/25C07C233/15C07C233/14
Inventor 祁昕欣包志鹏缪仁冠吴小锋
Owner ZHEJIANG SCI-TECH UNIV
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