Prop-2-yn-1-yl1H-imidazole-1-carboxylate synthesis
- Product Name:Prop-2-yn-1-yl1H-imidazole-1-carboxylate
- CAS Number:83395-38-4
- Molecular formula:C7H6N2O2
- Molecular Weight:150.13
288-32-4
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Yield:83395-38-4 94%
Reaction Conditions:
Stage #1: phosgene;propargyl alcohol at -8 - 5;Flow reactor;
Stage #2: 1H-imidazolewith triethylamine in dichloromethane; for 6 h;Inert atmosphere;Reflux;Temperature;
Steps:
4.I-4.II; 5.I-5.II; 6.I-6.II Example 4
I. Using 56g propynyl alcohol as raw material, cooling to -8°C, and injecting phosgene into the reaction kettle at a rate of 50 mL/min, and controlling the temperature of the reaction kettle to be less than 5°C during the process of introducing phosgene to carry out the reaction, TLC Monitor the progress of the reaction. After the reaction is over, keep it warm for 30 minutes, and then pour nitrogen into the reactor for 1.5 hours at room temperature, distill under reduced pressure, and collect 118°C fractions.Obtain 113.79g of distillate for use, with a yield of 96%;II. Add 174.28ml of dichloromethane and 43.57g of imidazole to the reaction kettle, add 106.46ml of triethylamine to the reaction kettle at a rate of 100mL/min, after the addition, replace the gas in the reaction kettle with nitrogen, and heat to reflux temperature , Add the fractions collected in step I dropwise to the reaction kettle, dripping for 1h, after dripping, stirring for 5h, suction filtration, the filter cake is washed with dichloromethane, the separated mother liquor is washed with lye to pH 7.3, with no Water magnesium sulfate is dried and distilled under reduced pressure,Obtained 135.50g product with a yield of 94%; the lye is an aqueous sodium bicarbonate solution with a concentration of 10g/L, as shown in Figure 4-6.Using mass spectrum, H spectrum and C spectrum to identify the product obtained as 2-propyn-1-yl 1H-imidazole-1-carboxylate,The structural formula of 2-propyn-1-yl 1H-imidazole-1-carboxylate is:
References:
CN112778205,2021,A Location in patent:Paragraph 0035-0043
288-32-4
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83395-38-4
52 suppliers
$80.09/5g