HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 67052701, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | (5-Amino-6-methoxypyridin-2-yl)dimethylphosphine oxide | HCID 67052694 | — |
| Reactant | HCID 86668812 | HCID 86668812 | — |
| Solvent | Ethanol | HCID 702 | — |
| Solvent | 2-Methoxyethanol | HCID 8019 | — |
| Product | HCID 67052701 | HCID 67052701 | — |
Reaction Steps
To a solution of 6-chloro-N-[2-(propan-2-ylsulfonyl)phenyl]pyrimidin-4-amine (0.250 mmol) in 1 mL of 2-methoxyethanol is added 6-(dimethylphosphoryl)-2-methoxypyridin-3-ylamine (50.0 mg, 0.250 mmol) and 0.15 mL of 2.5 M HCl in ethanol. The mixture is heated in a sealed tube at 90° C. until formation of the desired compound. The mixture is basified with 1N NaOH solution, and extracted with ethyl acetate. The organic layers can be combined, washed with saturated sodium chloride solution, dried with sodium sulfate, filtered and concentrated. The crude residue can be purified by silica gel chromatography.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09273077B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-d1189b878d1a4f85b7c700e45a094f87 |
| Source note | uspto-grants-2016_03 |