2-Propenoic acid, 2,3-dimethoxy-, methyl ester, (Z)- (9CI) synthesis
- Product Name:2-Propenoic acid, 2,3-dimethoxy-, methyl ester, (Z)- (9CI)
- CAS Number:59034-36-5
- Molecular formula:C6H10O4
- Molecular Weight:146.14
107-31-3
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Yield:59034-36-5 91.7%
Reaction Conditions:
with potassium-t-butoxide in tetrahydrofuran at -5 - 30; for 12 h;Inert atmosphere;Reagent/catalyst;
Steps:
1-2 Synthesis of Compound (Z)-methyl 2,3-dimethoxyacrylate (b1)
The compound of formula a1 (12.12 g, 115.2 mmol), methyl formate (8.74 g, 138.3 mmol) and tetrahydrofuran (500 mL) were mixed, replaced with nitrogen, and cooled to -5 to 5 °C to a colorless and clear system. t-BuOK (18.08 g, 161.2 mmol) was added, and the system was an off-white suspension; the temperature was raised to 20-30 °C, stirred for more than 12 h, water (500 mL) was added at 0-10 °C, stirred for 30 min, and ethyl acetate (1000 mL) was added for extraction, separated to obtain the aqueous phase, extracted with ethyl acetate (500 mL), combined the organic phases, washed with salt, dried, and concentrated to obtain 15.44 g of the compound of formula b1 with a yield of 91.7%.
References:
CN114751902,2022,A Location in patent:Paragraph 0056-0059; 0071-0072
