HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diethyl Ether → 4-[4-Amino-6-(5-chloro-2-methyl-phenyl)-[1,3,5]triazin-2-ylamino]-benzaldehyde
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diethyl Ether | HCID 3283 | — |
| Reactant | {4-[4-Chloro-6-(5-chloro-2-methyl-phenyl)-[1,3,5]triazin-2-ylamino]-phenyl}-methanol | HCID 86588970 | — |
| Reactant | HCID 178418287 | HCID 178418287 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | 4-[4-Amino-6-(5-chloro-2-methyl-phenyl)-[1,3,5]triazin-2-ylamino]-benzaldehyde | HCID 10290989 | 7% |
Reaction Steps
To a suspension of the title compound of Example 41 (375 mg, 1.1 mmol) in dichloromethane (100 ml) was added pyridinium chlorochromate (810 mg, 2.7 mmol) and crushed molecular sieves (1.25 g, 3A). After stirring for 6 hours, diethyl ether (150 ml) was added and the mixture was filtered through a pad of silica gel under suction. The filtrate was concentrated under reduced pressure and purified by flash chromatography on silica gel eluting with ethyl acetate-hexane (1:3 followed by 1:2 followed by 1:1) to provide the title compound (25 mg, 7% yield). 1H NMR (DMSO-d6) 10.10 (s, 1H), 9.86 (s, 1H), 8.07 (d, J=8.6 Hz, 2H), 7.84 (d, J=8.6 Hz, 2H), 7.79 (s, 1H), 7.43 (m, 2H), 7.34 (m, 2H), 2.53 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07618968B2 |
| Source dataset | uspto-grants-2009_11 |
| ORD ID | ord-c375d4849178412b8077f89cf867ce6e |
| Source note | uspto-grants-2009_11 |