HuagongsheHuagongshe Chemistry Print Report · For research reference only
4,6-Dichloropyrimidine → HCID 54594436, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4,6-Dichloropyrimidine | HCID 70943 | — |
| Reactant | Cyclopropanemethanamine | HCID 75646 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | HCID 54594436 | HCID 54594436 | 95.3% |
Reaction Steps
In a microwave reaction vessel, slurry 4,6-dichloropyrimidine (540 mg, 3.6 mmol), cyclopropylmethylamine (2800 L, 3.24 mmol), and diisopropylethylamine (1.25 mL, 7.2 mmol) in iso-propanol (3 mL). Irradiate in microwave (300 watts) at 140° C. for 40 min. Cool to room temperature and concentrate in vacuo. Purify by chromatography on silica gel (40 g) eluting with hexane/EtOAc (9:1 to 3:1 over 30 min; 40 mL/min) to obtain the desired intermediate (567 mg, 86%) as an off-white solid. MS (ES+) m/z: 184 (M+H)+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08680091B2 |
| Source dataset | uspto-grants-2014_03 |
| ORD ID | ord-300afed28ee9431cacaeac404966720a |
| Source note | uspto-grants-2014_03 |