HuagongsheHuagongshe Chemistry Print Report · For research reference only
Carbon Tetrachloride → HCID 68801608, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Carbon Tetrachloride | HCID 5943 | — |
| Reactant | Triphenylphosphine | HCID 11776 | — |
| Reactant | HCID 68801860 | HCID 68801860 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 68801608 | HCID 68801608 | — |
Reaction Steps
To the solution of 3-{hydroxy[2-(methylthio)pyrimidin-4-yl]methyl}benzonitrile (1.65 g, 6.41 mmol) in CCl4 (10 mL) and CH2Cl2(10 mL) was added triphenylphophine (2.36 g, 8.98 mmol) and stirred for 4 h. The mixture was concentrated and the residue was purified by silica gel chromatography (20% EtOAc in hexane) to give 3-{chloro[2-(methylthio)pyrimidin-4-yl]methyl}benzonitrile. 1H-NMR (500 MHz, CDCl3) δ 8.58 (d, 1H, J=5.1), 7.79 (s, 1H), 7.70 (d, 1H, J=8.1), 7.62 (d, 1H, J=7.8), 7.49 (t, 1H, J=7.8), 7.25 (d, 1H, J=4.9), 5.92 (s, 1H), 2.51 (s, 3H). LRMS m/z (M+H) Calcd: 276.8, found: 276.0.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07569589B2 |
| Source dataset | uspto-grants-2009_08 |
| ORD ID | ord-c20f014a640b4e228fb1d5efafef0bb6 |
| Source note | uspto-grants-2009_08 |