3,4-Difluoro-N-methylbenzenemethanamine synthesis
- Product Name:3,4-Difluoro-N-methylbenzenemethanamine
- CAS Number:748124-46-1
- Molecular formula:C8H9F2N
- Molecular Weight:157.16
Yield:748124-46-1 92%
Reaction Conditions:
in tetrahydrofuran at 0 - 15; for 12 h;Inert atmosphere;
Steps:
I.1 Intermediate compound 43:
To a solution of MeML (2 M, 7.25 mL, 14.5 mmol) in THF (6.0 mL) was added 4-(bromom ethyl)- 1,2-difluorobenzene (0.5 g, 2.42 mmol) at 0°C under N2. The mixture was stirred at 15 °C for 12 hrs; The reaction mixture was washed with a saturated solution of NaHCCh (50 mL) and extracted with ethyl acetate (20 mL, 3 times). The combined organic layers were washed with brine (50 mL), dried over Na2SC>4, filtered and concentrated under reduced pressure to give the Intermediate compound 43 (0.35 g, yield 92 %) as yellow oil. LCMS (ESI position ion) m/z: (M+H)+: 157.9 (calculated: 158.1). NMR (ET34313-2-P1A, CDCh-d, 400 MHz) d = 7.14 - 7.07 (m, 2H), 7.04 - 7.03 (m, 1H), 3.71 (s, 2H), 2.44 (s, 3H).
References:
WO2021/170797,2021,A1 Location in patent:Page/Page column 134; 157
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