Methanesulfonic Acid → HCID 22667440, compound

HRID 1007055Notes

Reaction equation

[F:1][C:2]1[C:3]([CH:25]=[CH:26]OC)=[C:4]([C:10]2[CH:15]=[CH:14][C:13]([CH:16]3[CH2:21][CH2:20][CH:19]([CH2:22][CH2:23][CH3:24])[CH2:18][CH2:17]3)=[CH:12][CH:11]=2)[CH:5]=[C:6]([F:9])[C:7]=1[F:8].CS(O)(=O)=O>ClCCl>[F:1][C:2]1[C:3]2[CH:25]=[CH:26][C:15]3[C:10](=[CH:11][CH:12]=[C:13]([CH:16]4[CH2:21][CH2:20][CH:19]([CH2:22][CH2:23][CH3:24])[CH2:18][CH2:17]4)[CH:14]=3)[C:4]=2[CH:5]=[C:6]([F:9])[C:7]=1[F:8]

Participants

Conditions

Temperature: 0 °C

Procedure

6.1 g of 3,4,5-trifluoro-2-(2-methoxyvinyl)-4′-(4-propylcyclohexyl)biphenyl are dissolved in 180 ml of dichloromethane, and 8.5 ml of methanesulfonic acid are added at 0° C. After the reaction mixture has been stirred at 0° C. for 2.5 hours, it is added to ice-water and subjected to conventional work-up. Chromatographic purification (silica gel, n-heptane) and recrystallisation from n-heptane gives 1,2,3-trifluoro-7-(4-propylcyclohexyl)phenanthrene in the form of colourless crystals. C: 124, N: 124.4, I; Δε=12.7; Δn=0.1843;

Workup

customChromatographic purification (silica gel, n-heptane) and recrystallisation from n-heptane

Sources & evidence

ORD record: ord-3be39a2d1c2a4f018c4ac5af35fc0e0a
Source dataset: uspto-grants-2004_09
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US06793984B2

Reaction notes

Loading…