HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → HCID 178482085, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | Methylamine | HCID 6329 | — |
| Reactant | HCID 178509408 | HCID 178509408 | — |
| Product | HCID 178482085 | HCID 178482085 | 44% |
Reaction Steps
A solution of 4-(2,4-dichlorophenyl)-2-(2-fluoropyridin-4-yl)-5-(4H-1,2,4-triazol-3-yl)thiophene-3-carbonitrile (0.100 g, 0.000240 mol) and 1M Methylamine in methanol (4 mL, 0.004 mol) 0.000163 mol) was heated at 80° C. for 5 hours. The solvent was removed and the residue was purified using a silica gel chromatography (12 g), elution DCM to 5% MeOH in DCM over 20 minutes to afford the title compound (0.045 g, 44%). LCMS: (FA) ES+, 427, 429. 1H NMR (400 MHz, d4-Methanol) 8.38 (s, 1H), 8.12-8.07 (m, 1H), 7.60 (dd, J=1.56, 0.77 Hz, 1H), 7.44-7.42 (m, 2H), 6.94 (dd, J=4.67, 1.66 Hz, 1H), 6.93 (s, 1H), 2.92 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09139589B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-b7e1b2fe5a4b49d89dadd273bf610db0 |
| Source note | uspto-grants-2015_09 |