1,3-Benzodioxole-5-carboxylic acid ethyl ester synthesis
- Product Name:1,3-Benzodioxole-5-carboxylic acid ethyl ester
- CAS Number:6951-08-2
- Molecular formula:C10H10O4
- Molecular Weight:194.18
Yield:6951-08-2 59%
Reaction Conditions:
Stage #1: Piperonylic acidwith oxalyl dichloride in dichloromethane at 20; for 1 h;
Stage #2: ethanolwith triethylamine in dichloromethane at 20; for 1.5 h;Cooling with ice;
Steps:
2.2 2) Synthesis of benzo[1,3]dioxole-5-carboxylic acid ethyl ester(P-6)
Weigh compound P-5 (100 mg, 0.6 mmol) Resuspended in 5 mL of dry CH2Cl2 Addition of oxalyl chloride (76mg, 0.6mmol) And 2mL dry CH2Cl2 solution, After the addition, the mixture was stirred at room temperature for 1 h. After 1 hour, the solvent was distilled off under reduced pressure. Dissolved in 5 mL of dry CH2Cl2 In an ice bath was added dropwise from anhydrous ethanol (139 mg, 3 mmol), A solution consisting of triethylamine (183 mg, 1.8 mmol) and 5 mL of dry CH2Cl2 was added. Add about 30min, After the addition, react at room temperature for 1 hour. Pour into ice water, Extraction with ethyl acetate (50 mL × 2) The organic phase was washed twice with water and dried over anhydrous Na2SO4 overnight. Filtering, Concentrated white oil, Separation with 300-400 mesh silica gel column chromatography, The eluent was n-hexane:ethyl acetate=10:1 (v/v) to give 69 mg of a white oil. After curing, yield 59%.
References:
CN104016960,2018,B Location in patent:Paragraph 0103-0106; 0111-0113
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