HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dimethoxyethane → 4-Chloro-6-(2-methoxyphenyl)pyrimidine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dimethoxyethane | HCID 8071 | — |
| Reactant | 4,6-Dichloropyrimidine | HCID 70943 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | 2-Methoxyphenylboronic acid | HCID 2733958 | — |
| Catalyst | HCID 178418476 | HCID 178418476 | — |
| Solvent | Water | HCID 962 | — |
| Product | 4-Chloro-6-(2-methoxyphenyl)pyrimidine | HCID 15206835 | 75% |
Reaction Steps
4,6-dichloropyrimidine (6.0 g, 40 mmol) and 2-methoxyphenylboronic acid (4.41 g, 29 mmol) were added to a solution of dimethoxyethane (120 mL) and water (18 mL), followed by the addition of NaHCO3 (6.72 g, 80 mmol) and (PPh3)2PdCl2 (0.84 g). to this end the reaction mixture was allowed to reflux for 8 h, and then the solvent removed under reduced pressure. The residue was taken up in CH2Cl2 (100 mL), and the resulting solution washed with water, dried over anhydrous K2CO3, filtered and the solvent removed under reduced pressure. The crude product was purified by flash chropatography on silica gel (eluent CH2Cl2) and recrystallized from hexanes yielding 4-chloro-6-(2-methoxyphenyl)-pyrimidine (4.78 g; 75%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08507498B2 |
| Source dataset | uspto-grants-2013_08 |
| ORD ID | ord-064a91968a374aeaa3c28cfb943baa0c |
| Source note | uspto-grants-2013_08 |