HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 9943499, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 9943500 | HCID 9943500 | — |
| Solvent | Diethyl Ether | HCID 3283 | — |
| Product | HCID 9943499 | HCID 9943499 | 47% |
Reaction Steps
4,6-Dimethoxy-2-(phenylethynyl)pyrimdine (320 mg, 1.3 mmol) was dissolved in CH2Cl2 (1.0 mL), and treated with HCI in diethyl ether (1.6 mL of a 1.0M solution, 1.6 mmol). A yellow solid precipitated immediately. The mixture was diluted with ethyl acetate and allowed to stand in the freezer for 16 h. The cold supernatant was decanted and the remaining solids were triturated with ethyl acetate (1.5 mL), and then hexane (3.times.2 mL). The remaining solid was dried in vacuo to afford 4,6-dimethoxy-2-(phenylethynyl)pyrimdine hydrochloride (174 mg, 47% yield) as a yellow solid. M.p. 137-138. 1H NMR (CD3OD, 300 MHz) Δ7.65-7.62 (m, 2H), 7.46-7.42 (m, 3H), 6.16 (s, 1H), 3.97 (s, 6H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07462619B2 |
| Source dataset | uspto-grants-2008_12 |
| ORD ID | ord-d56ea2a24ffc4927812963cf1edcaaf8 |
| Source note | uspto-grants-2008_12 |