2-fluoro-3-methylbut-2-enoic acid synthesis
- Product Name:2-fluoro-3-methylbut-2-enoic acid
- CAS Number:15051-86-2
- Molecular formula:C5H7FO2
- Molecular Weight:118.11
685-89-2
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15051-86-2
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Yield:15051-86-2 99.9%
Reaction Conditions:
with lithium hydroxide monohydrate in tetrahydrofuran;methanol at 0 - 50; for 12 h;
Steps:
1.2 Step 2:
To a solution of intermediate 2 (2.68 g, 18.2 mmol) in MeOH (8 mL), THF (8 mL) and water (8 mL) was added LiOH·H2O (3.8 g, 91.2 mmol) at 0 °C. The mixture was stirred at 50 °C for 12 hours. The mixture was concentrated to 1/5 volume, diluted with water and washed with MTBE twice. The aqueous layer was acidified with IN aq.HCl to pH = 3, extracted with DCM twice. The combined organic layers were washed with brine, dried over anhydrous Na2SO4, and concentrated under reduced pressure to dryness to give intermediate 3 (2.16 g, yield 99.9%) as a white solid. LC/MS (ESI) (m/z) : 119 (M+H)+.
References:
WO2021/168320,2021,A1 Location in patent:Paragraph 112; 148-149
