The Instruction of Methyl 5-chloropyrazine-2-carboxylate

Introduction

Methyl 5-chloropyrazine-2-carboxylate is an organic compound that is used as an intermediate in the production of various chemicals, pharmaceuticals, and agrochemicals.
The synthesis of this compound involves several steps, and the instructions for carrying out these steps are critical to ensure that the final product is of high quality and purity.
In this article, we will discuss the instructions for the synthesis of methyl 5-chloropyrazine-2-carboxylate, including the materials and equipment required, the steps involved, and the precautions that must be taken to ensure success.

Materials and Equipment Required

The synthesis of methyl 5-chloropyrazine-2-carboxylate requires a range of materials and equipment, including:

1. Chloroform
2. Sodium hydroxide
3. Ethyl acetate
4. 5-chloropyrazine-2-carboxylic acid
5. Methyl iodide
6. Ice
7. Water
8. Filter paper
9. Glass beads
10. Vacuum pump
11. Thermometer
12. Magnetic stirrer

Steps Involved

The synthesis of methyl 5-chloropyrazine-2-carboxylate involves several steps, including:

Step 1: Preparation of 5-chloropyrazine-2-carboxylic acid

To prepare 5-chloropyrazine-2-carboxylic acid, 200 mL of chloroform is added to a 500-mL round-bottom flask equipped with a magnetic stirrer and a thermometer.
2.
5 g of sodium hydroxide is then added to the chloroform, and the mixture is stirred for 30 minutes at room temperature.
The mixture is then cooled to 0°C, and a solution of 2.
5 g of 5-chloropyrazine-2-carboxylic acid in 50 mL of ethyl acetate is added dropwise over a period of 1 hour.
The mixture is then stirred for a further 30 minutes, and the resulting slurry is filtered through filter paper using glass beads and vacuum pump.
The resulting filtrate is then washed with 50 mL of ice-cold water and 50 mL of ice-cold 1% aqueous sodium carbonate solution, and the organic layer is separated and dried over anhydrous sodium sulfate.
The filtrate is then concentrated under reduced pressure, and the resulting solid is dried under high vacuum for 2 hours to afford 5-chloropyrazine-2-carboxylic acid as a white solid.

Step 2: Methylation of 5-chloropyrazine-2-carboxylic acid

To methylate 5-chloropyrazine-2-carboxylic acid, a solution of 1.
0 g of 5-chloropyrazine-2-carboxylic acid in 50 mL of methylene chloride is added to a 100-mL round-bottom flask equipped with a magnetic stirrer and a thermometer.
1.
5 mL of methyl iodide is then added to the solution, and the mixture is stirred for 30 minutes at room temperature.
The mixture is then cooled to 0°C, and 10 mL of ice is added.
The mixture is then stirred for a further 30 minutes, and the resulting slurry is filtered through filter paper using glass beads and vacuum pump.
The resulting filtrate is then washed with 10 mL of ice-cold water