2-Propen-1-one, 1-(3,4-difluorophenyl)-3-(dimethylamino)-, (2E)- synthesis
- Product Name:2-Propen-1-one, 1-(3,4-difluorophenyl)-3-(dimethylamino)-, (2E)-
- CAS Number:1613411-77-0
- Molecular formula:C11H11F2NO
- Molecular Weight:211.21
Yield:1613411-77-0 99%
Reaction Conditions:
in N,N-dimethyl-formamide; for 22 h;Reflux;
Steps:
1.1 Step 1
l-(3,4-difluorophenyl)ethan-1-one (1000 mg, 6.41 mmol) and DMF-DMA (3.40 mL, 25.62 mmol) were combined in DMF (3 mL) and heated to reflux for 22 hr. The mixture was extracted by DCM and aq. NH4C1. The organic layer was dried over anhydrous MgSO4 and concentrated to give (E)-1-(3,4-difluorophenyl)-3-(dimethylamino)prop-2-en-1-one (1275.4 mg, >99%) as an orange solid. 1HNMR(400 MHz, DMSO-d6 δ 7.96 - 7.88 (m, 1H), 7.82 - 7.77 (m, 1H), 7.74 (d, J = 12.2 Hz, 1H), 7.53 - 7.45 (m, 1H), 5.85 (d, J = 12.2 Hz, 1H), 3.15 (s, 3H), 2.93 (s, 3H).
References:
WO2022/84741,2022,A1 Location in patent:Paragraph 00341; 00350