HuagongsheHuagongshe Chemistry Print Report · For research reference only
Methanol → 4-[4-Methyl-2-[(7-methylpyrido[2,3-d]pyrimidin-4-yl)amino]phenyl]sulfanylphenol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Methanol | HCID 887 | — |
| Reactant | 4-(2-Amino-4-methyl-phenylsulfanyl)-phenol | HCID 66808123 | — |
| Reactant | N'-(3-Cyano-6-methyl-pyridin-2-yl)-N,N-dimethyl-formamidine | HCID 66808573 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Product | 4-[4-Methyl-2-[(7-methylpyrido[2,3-d]pyrimidin-4-yl)amino]phenyl]sulfanylphenol | HCID 57393153 | 56% |
Reaction Steps
To a solution of the product from Example 10B (100 mg, 0.575 mmol) and the product from Example 9c (146 mg, 0.632 mmol) in acetic acid (1 mL) was heated at 130° C. for 1 hour. The mixture was then allowed to cool to room temperature, then methanol (5 mL) added to the solution and the resulting solid collected and washed with methanol to provide the title compound (120 mg, 56%). 1H NMR (300 MHz, DMSO-D6) δ ppm: 2.29 (s, 3H), 2.66 (s, 3H), 6.73 (d, J=8.8 Hz, 2H), 6.93 (m, 1H), 7.03 (m, 1H), 7.18 (d, J=8.5 Hz, 2H), 7.26, (s, 1H), 7.53 (d, J=8.5 Hz, 1H), 8.53 (s, 1H), 8.77 (m, 1H), 9.76 (bs, 1H), 9.96 (bs, 1H); MS (ESI)+ m/z 375 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08236950B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-46a8f60316af41caa83c5a1db91df387 |
| Source note | uspto-grants-2012_08 |