HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 4-[(5-Chloro-2,6-dimethylpyrimidin-4-ylamino)methyl]-2-methoxyphenol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | (4-Benzyloxy-3-methoxybenzyl)(5-chloro-2,6-dimethylpyrimidin-4-yl)amine | HCID 22640039 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 4-[(5-Chloro-2,6-dimethylpyrimidin-4-ylamino)methyl]-2-methoxyphenol | HCID 22640008 | 60.2% |
Reaction Steps
In analogy to the method described in example B1, 3.0 g (7.8 mmol) of (4-benzyloxy-3-methoxy-benzyl)(5-chloro-2,6-dimethylpyrimidin-4-yl)amine (from example A3) are reacted with 30 ml of 12.5N hydrochloric acid in 30 ml of ethanol. Extraction with ethyl acetate at a pH of 8 gives, after concentration, a solid residue which is chromatographed on silica gel (mobile phase: toluene/dioxane=5:1). Crystallization with toluene gives 1.38 g (60%) of the title compound as a beige crystallizate. m.p.: 179-181.5° C.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06818642B2 |
| Source dataset | uspto-grants-2004_11 |
| ORD ID | ord-e84ab9daeb2c425b894178571f27cc9c |
| Source note | uspto-grants-2004_11 |