HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → HCID 67517677, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | HCID 86706479 | HCID 86706479 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 67517677 | HCID 67517677 | 35% |
Reaction Steps
To a mixture of N-(2-(2-(3,5-dichlorophenylamino)acetyl)-1,2,3,4-tetrahydroisoquinolin-4-yl)-2,2,2-trifluoroacetamide (0.45 g, 1.0 mmol), in aq. MeOH (15 mL) was added K2CO3 (1.0 g, 6.0 mmol) and the reaction mixture was heated to reflux for 2.5 h. The reaction mixture was concentrated in vacuo to give a residue which was purified by column chromatography (silica gel, gradient MeOH in DCM) to give (0.120 g, 35%) of the titled intermediate. 1H NMR (DMSO-d6, 400 MHz): δ 7.30-7.19 (m, 3H), 7.05-6.95 (m, 1H), 9.71 (s, 1H), 6.45 (d, 2H, J=11.2 Hz), 5.19 (d, J=8.0 Hz, 1H), 4.65 (s, 1H), 4.89-3.99 (m, 2H), 3.85-3.69 (m, 3H), 3.3-3.2 (m, 2H). LCMS: M/z: (M+1):350
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09273028B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-b65135de0b4f4a28a239d3eca10386f9 |
| Source note | uspto-grants-2016_03 |