HuagongsheHuagongshe Chemistry Print Report · For research reference only
Chloroform → HCID 57428967, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Chloroform | HCID 6212 | — |
| Reactant | Hexane | HCID 8058 | — |
| Reactant | Phosphorus oxychloride | HCID 24813 | — |
| Reactant | HCID 57428968 | HCID 57428968 | — |
| Solvent | Acetic Anhydride | HCID 7918 | — |
| Product | HCID 57428967 | HCID 57428967 | — |
Reaction Steps
4-Chloro-2,6-dimethylfuro[2,3-d]pyrimidine (M).To a 50 mL flask was added 1.64 g (1 mmol) L and 10 mL POCl3. The resulting mixture was refluxed for 2 h, and the solvent was removed under reduced pressure to afford a dark residue. To this was added 30 mL of CHCl3 and 3 g of silica gel. The solvent was evaporated to afford a plug. Column chromatography of the plug with hexane:acetyl acetate=20:1 as eluent afford 1.55 g (85%) M as a yellow solid; Rf 0.26 (Hexane/EtOAC 15:1); 1H NMR (DMSO-d6) δ 2.48 (s, 3 H), 2.63 (s, 3 H), 6.77 (s, 1 H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09139590B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-9412d787c3bf4a188e9a06863f64dc80 |
| Source note | uspto-grants-2015_09 |