HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Amino-4,6-dichloropyrimidine → HCID 58504602, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Amino-4,6-dichloropyrimidine | HCID 65522 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | (3R)-3-Ethylmorpholine | HCID 14267783 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 58504602 | HCID 58504602 | 86.6% |
Reaction Conditions
| Temperature | 150 °C |
|---|
Reaction Steps
To 4,6-dichloro-2-pyrimidinamine (240 mg, 1.46 mmol) in CH3CN (8 mL) were added (3R)-3-ethylmorpholine (244 mg, 1.61 mmol) and Hunig's base (1.02 mL, 5.85 mmol), and the reaction mixture was heated in a microwave at 150° C. for a total of 3 hours, checking the progression of the reaction at regular intervals. The mixture was evaporated under vacuum, and the resulting residue was partitioned between EtOAc and water. The aqueous layer was extracted with EtOAc (2×) and CH2Cl2 (2×). The organics were washed with water and brine, dried (MgSO4), filtered and evaporated. The resulting material was triturated with Et2O and dried in vacuo to afford the title compound (307 mg). LC-MS (ES) m/z=243, 245 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08697685B2 |
| Source dataset | uspto-grants-2014_04 |
| ORD ID | ord-ef93fe14888749f2b221a66b05d35c3e |
| Source note | uspto-grants-2014_04 |