HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chloro-4-hydroxybenzaldehyde → HCID 69707946, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chloro-4-hydroxybenzaldehyde | HCID 185363 | — |
| Reactant | 4-(3-Chloro 4-fluoro-phenylamino)-5,7-dihydro-pyrrolo[2,3-d]pyrimidin-6-one | HCID 9878769 | — |
| Catalyst | Piperidine | HCID 8082 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 69707946 | HCID 69707946 | — |
Reaction Steps
The mixture of 4-(3-chloro-4-fluoro-phenylamino)-5,7-dihydro-pyrrolo[2,3-d]pyrimidin-6-one (100 mg, 0.36 mmol), 2-chloro-4-hydroxy-benzaldehyde (84.5 mg, 0.54 mmol), and piperidine (3 drops), in ethanol (3 mL) was heated at 60° C. oil bath for 4 hours, and cooled to room temperature. The product was crystallized out, filtered, washed by ethanol, and dried under high vacuum to provide pure 4-(3-chloro-4-fluoro-phenylamino)-5-[-(2-chloro-4-hydroxy-phenyl)-methylidene]-5,7-dihydro-pyrrolo[2,3-d]pyrimidin-6-one. 1H NMR (400 MHz, DMSO-d6) d 11.52 (br s, 1H), 10.45 (br s, 1H), 8.42 (s, 1H), 8.35 (br s, 1H), 7.65 (s, 1H), 7.11 (t, 1H), 6.96 (m, 1H), 6.79 (m, 1H), 6.72 (d, 1H), 6.66 (m, 1H), 6.56 (dd, 1H). MS 418 [M++1].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06908930B2 |
| Source dataset | uspto-grants-2005_06 |
| ORD ID | ord-a8c8bcbf1aec4ba9a79d089b6b011b23 |
| Source note | uspto-grants-2005_06 |