METHYL 5-FORMYL-2-METHYL-3-FUROATE synthesis
- Product Name:METHYL 5-FORMYL-2-METHYL-3-FUROATE
- CAS Number:81661-26-9
- Molecular formula:C8H8O4
- Molecular Weight:168.15
6141-58-8
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Yield:81661-26-9 83%
Reaction Conditions:
with trichlorophosphate in N,N-dimethyl-formamide at 0 - 100; for 3 h;
Steps:
Step 1: Methyl 5-formyl-2-methylfuran-3-carboxylate
POCl3 (1.09 g, 7.14 mmol, 663.12 uL) was added to DMF (678.57 mg, 9.28 mmol, 714.29 uL) dropwise at 0 °C. After stirring at 0 °C for 15 min, methyl 2-methylfuran-3- carboxylate (1.0 g, 7.14 mmol, 892.86 uL) was added to the mixture at 15 °C. The mixture was then stirred at 100 °C for 3 hrs. The mixture was poured onto 20 g of ice and the pH was adjusted to 8 with 10% aq. NaOH at 0-10 °C. The mixture was filtered. The filter solid was washed with H2O (5.0 mL × 3) and dried in vacuo to afford the title compound (1.0 g, 83%) as a yellow solid..1H NMR (400 MHz, DMSO-d6) d 9.56 (s, 1H), 7.47 (s, 1H), 3.87 (s, 3H), 2.69 (s, 3H).
References:
WO2021/7477,2021,A1 Location in patent:Page/Page column 77
15341-69-2
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![3-Furancarboxylic acid, 2-methyl-5-(1,2,3,4-tetrahydroxybutyl)-, methyl ester, [1S-(1R*,2S*,3S*)]- (9CI)](/CAS/20210305/GIF/17651-08-0.gif)
17651-08-0
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81661-26-9
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105-45-3
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