Example 13: Synthesis of 2,2-difluoroethanol from ethyl 2,2-difluoroacetate (Step b2)
In a 0.5 L glass reactor equipped with a mechanical stirrer, reflux condenser and temperature probe, 164 g of ethyl 2,2-difluoroacetate (GC purity 95%), 106 g of methanol, and 3 g of solid NaOH were added. the reaction was carried out at 65 °C for 2 h until the conversion was complete. The 2,2-difluoroethanol was isolated by distillation to give 96.3% GC purity and 87% isolated yield.
[1] Patent: CN107986944, 2018, A. Location in patent: Paragraph 0020; 0023; 0026; 0029; 0032
[2] Patent: WO2009/40367, 2009, A1. Location in patent: Page/Page column 12
[3] Patent: US2014/243561, 2014, A1. Location in patent: Paragraph 0040; 0041; 0042
[4] Patent: WO2009/40367, 2009, A1. Location in patent: Page/Page column 10
[5] Patent: CN108178723, 2018, A. Location in patent: Paragraph 0015; 0016; 0018; 0020