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A kind of preparation method of 4-(1-hydroxy-1-methylethyl)-2-propyl imidazole-5-carboxylic acid ethyl ester

A technology of propyl imidazole and methyl ethyl, which is applied in the field of synthesis of pharmaceutical intermediates, can solve problems such as leakage of volatile raw materials, affecting efficient and stable preparation, etc.

Active Publication Date: 2022-05-13
ZHEJIANG HUADEE DYESTUFF CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Although the above-mentioned patents can be used for ethyl 4-1-hydroxy-1-methylethyl-2-propyl-1H-imidazole-5-carboxylate; but when the existing preparation methods are making the above-mentioned substances, most of them A three-necked round-bottom flask is used for the mutual reaction of various solvents. Since solvents need to be continuously added to the three-necked round-bottom flask, and one of the feeding ports of the three-necked round-bottom flask needs to be exposed, the sealing plug needs to be continuously removed. , which in turn leads to volatile leakage of internal volatile raw materials, which in turn affects the efficient and stable preparation of ethyl 4-(1-hydroxy-1-methylethyl)-2-propylimidazole-5-carboxylate

Method used

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  • A kind of preparation method of 4-(1-hydroxy-1-methylethyl)-2-propyl imidazole-5-carboxylic acid ethyl ester
  • A kind of preparation method of 4-(1-hydroxy-1-methylethyl)-2-propyl imidazole-5-carboxylic acid ethyl ester
  • A kind of preparation method of 4-(1-hydroxy-1-methylethyl)-2-propyl imidazole-5-carboxylic acid ethyl ester

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preparation example Construction

[0028] Such as Figure 1-Figure 4 Shown, the preparation method of a kind of 4-(1-hydroxyl-1-methylethyl)-2-propylimidazole-5-carboxylate ethyl ester of the present invention, the method comprises the steps:

[0029] S1: first seal the three-necked round-bottom flask 2 into the cooling pot of the magnetic stirrer 1, and put the magnetic stirring block 3 into the three-necked round-bottomed flask 2 from the middle pipe 21 of the three-necked round-bottomed flask 2 through the air guide tube 4; Insert the feed pipe 22 on the left and right sides of the three-necked round bottom flask 2 into the reagent dropper 5 in a sliding seal;

[0030] S2: Fill 120 mL of tetrahydrofuran solution of methylmagnesium bromide into the rubber cap 6 of the detachable reagent dropper 5, then install the rubber cap 6 on the reagent dropper 5 on the left side of the three-necked round bottom flask 2, squeeze Press the rubber cap 6 to make the solution inside enter the three-necked round-bottomed fla...

Embodiment approach

[0036] As an embodiment of the present invention, the reagent dropper 5 is inserted into the feed pipe 22 through a sealing plug to slide and seal, and the top of the reagent dropper 5 is provided with an internal thread; the rubber cap 6 is fixed with an outer thread. threaded conduit 8, and the externally threaded conduit 8 is threadedly connected to the internal thread; during work, when the rubber cap 6 needs to be installed on the reagent dropper 5, the experimenter connects the externally threaded conduit 8 on the rubber cap 6 with the reagent dropper 5, and then rotate the rubber cap 6, so that the externally threaded conduit 8 can be threaded into the inside of the reagent dropper 5, thereby facilitating the fast fixing of the rubber cap 6 to the reagent dropper 5, and also facilitating the diversion and sealing The mechanism 7 can quickly open the rubber cap 6, so that the solvent inside the rubber cap 6 can enter the reagent dropper 5; at the same time, the experiment...

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Abstract

The invention belongs to the technical field of pharmaceutical intermediate synthesis, specifically a preparation method of 4-(1-hydroxyl-1-methylethyl)-2-propylimidazole-5-ethyl carboxylate; Magnesium bromide tetrahydrofuran solution 120mL is filled into the rubber cap of the detachable reagent dropper, and then the rubber cap is installed on the reagent dropper on the left side of the three-neck round bottom flask; Gas, simultaneously through the reagent dropper on the right side of the three-neck round-bottom flask, dropwise add 30mL of dichloromethane solution; the light yellow oily substance is dissolved in 10% 100mL of sodium hydroxide solution, add 2.0g of activated carbon powder, stir for 20min, and then Filtrate, cool the filtrate to 0°C with ice water, overnight, precipitate a large amount of solid, filter and dry to obtain solid 4-(1-hydroxyl-1-methylethyl)-2-propylimidazole-5-carboxylate ethyl ester ; Prevent the volatile raw materials inside the three-necked round-bottomed flask from volatilizing and leaking, thereby affecting the efficient preparation of -(-hydroxyl-methylethyl)-propylimidazole-ethyl carboxylate.

Description

technical field [0001] The invention belongs to the technical field of synthesis of pharmaceutical intermediates, in particular to a preparation method of ethyl 4-(1-hydroxyl-1-methylethyl)-2-propylimidazole-5-carboxylate. Background technique [0002] 4-(1-hydroxyl-1-methylethyl)-2-propylimidazole-5-ethyl carboxylate is used as a key intermediate in the synthesis of olmesartan medoxomil, and the quality of its synthesis process directly affects olmesartan Esters product quality and cost. The synthetic 4-(1-hydroxyl-1-methylethyl)-2-propylimidazole-5-carboxylate technique reported in most of the existing documents is all similar, all with 2-propylimidazole-4, It can be obtained by Grignard reaction between ethyl 5-dicarboxylate and methylmagnesium bromide, and quenching the reaction with ethyl acetate and saturated ammonium chloride. [0003] Chinese patent discloses a preparation method of 4-(1-hydroxyl-1-methylethyl)-2-propylimidazole-5-carboxylic acid ethyl ester, the p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J19/18B01J4/00C07D233/90
CPCB01J19/18B01J19/0053B01J19/0066B01J4/001C07D233/90
Inventor 顾敏伟
Owner ZHEJIANG HUADEE DYESTUFF CHEM