HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,4-Dichloropyrimidine → 2-chloro-N-(2,4,6-trifluorobenzyl)pyrimidin-4-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,4-Dichloropyrimidine | HCID 77531 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2,4,6-Trifluorobenzylamine | HCID 2777046 | — |
| Solvent | Isopropanol | HCID 3776 | — |
| Product | 2-chloro-N-(2,4,6-trifluorobenzyl)pyrimidin-4-amine | HCID 118155171 | — |
Reaction Steps
2,4,6-trifluorobenzylamine (5 g, 31 mmol) was added dropwise to a stirred suspension of 2,4-dichloropyrimidine (4.6 g, 31 mmol) and DIPEA (5.4 mL, 62 mmol) in IPA (100 mL) at 0° C. then the reaction mixture was warmed to room temperature and stirred overnight. The precipitate was collected and washed with diethyl ether to afford the first crop of 2-chloro-N-(2,4,6-trifluorobenzyl)pyrimidin-4-amine IV-1. The filtrate was concentrated and purified by column chromatography (0-30% v/v ethyl acetate/petrol) to afford a second crop (total yield 5.3 g, 62%). LC-MS (Method F), RT=2.27 min. (ES+) 274.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09296725B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-76dab07f299541c59727062031c6abfd |
| Source note | uspto-grants-2016_03 |