Synthesis and preparation method of 3-bromo-2, 2-dimethyl-1-propanol
A dimethyl and propanol technology is applied in the preparation of nitro compounds, the preparation of hydroxyl compounds, the preparation of organic compounds, etc., which can solve the problems of high cost and long reaction time, and achieves low environmental protection pressure, simple operation, and production cycle. short effect
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[0023] A kind of synthetic preparation method of 3-bromo-2,2-dimethyl-1-propanol, described method comprises the steps:
[0024] Step 1: Mix sodium nitrite, isopropanol and paraformaldehyde to generate 2-nitro-2-methyl-1-propanol:
[0025] Dissolve 1 part of isopropanol, 1 to 3 parts of paraformaldehyde, and 3 to 9 parts of sodium nitrite in water to obtain an aqueous solution;
[0026] Control the temperature of the aqueous solution at 3-14°C, and continue the reaction for 5-13 hours to obtain 2-nitro-2-methyl-1-propanol;
[0027] Step 2: Pass hydrogen and methane into 2-nitro-2-methyl-1-propanol to react to generate 2-2-dimethyl-1-propanol:
[0028] At room temperature, place 2-nitro-2-methyl-1-propanol in an airtight container and pass in hydrogen gas, and let it stand for 1 to 2 hours;
[0029] Raise the temperature to 50-80°C, feed methane, control the pressure at 2-5 Pa, and continue the reaction for 4-8 hours to obtain 2-2-dimethyl-1-propanol;
[0030] Wherein, the w...
Embodiment 1
[0038] Dissolve 1 part of isopropanol, 1 part of paraformaldehyde and 3 parts of sodium nitrite in water to obtain an aqueous solution;
[0039] The temperature of the aqueous solution was controlled at 3°C, and the reaction was continued for 5 hours to obtain 2-nitro-2-methyl-1-propanol;
[0040] At room temperature, place 2-nitro-2-methyl-1-propanol in an airtight container and pass through hydrogen gas, and let stand for 1h;
[0041] Raise the temperature to 50°C, feed methane, control the pressure at 2 Pa, and continue the reaction for 4 hours to obtain 2-2-dimethyl-1-propanol;
[0042] Wherein, the weight ratio of the 2-nitro-2-methyl-1-propanol, hydrogen and methane is 1:2:4;
[0043] Add sodium bromide to 2-2-dimethyl-1-propanol to react, react under light environment, control the reaction temperature at 30°C, and control the time at 6h, and the reaction will give 3-bromo-2-2-dimethyl Base-1-propanol;
[0044] Wherein, the weight ratio of the bromide to the peroxide ...
Embodiment 2
[0046] Dissolve 1 part of isopropanol, 2 parts of paraformaldehyde and 4 parts of sodium nitrite in water to obtain an aqueous solution;
[0047] The temperature of the aqueous solution was controlled at 5°C, and the reaction was continued for 8 hours to obtain 2-nitro-2-methyl-1-propanol;
[0048] At room temperature, place 2-nitro-2-methyl-1-propanol in an airtight container and pass through hydrogen gas, and let stand for 1h;
[0049] Raise the temperature to 60°C, feed methane, control the pressure at 3 Pa, and continue the reaction for 5 hours to obtain 2-2-dimethyl-1-propanol;
[0050] Wherein, the weight ratio of the 2-nitro-2-methyl-1-propanol, hydrogen and methane is 1:2:4;
[0051] Add hydrobromic acid to 2-2-dimethyl-1-propanol to react, and react under the environment of hydrogen peroxide. The reaction temperature is controlled at 40°C, and the time is controlled at 7h. The reaction gives 3-bromo-2-2-dimethyl Base-1-propanol;
[0052] Wherein, the weight ratio o...
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