HuagongsheHuagongshe Chemistry Print Report · For research reference only
Pyridine → HCID 10804547, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Pyridine | HCID 1049 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 10565203 | HCID 10565203 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 10804547 | HCID 10804547 | 165.6% |
Reaction Steps
Pyridine (79 mL, 0.97 mmol) was added to a stirring mixture of 8b (112 mg, 0.39 mmol) and triphosgene (46 mg, 0.16 mmol) in CH2Cl2 (5 mL) at r.t. After 15 minutes, the reaction mixture was concentrated in vacuo. Flash chromatography (20 g, 5:1 hexanes/ethyl acetate) yielded 9b (81 mg, 68%) as a white solid: 1H NMR (270 MHz, CDCI3) d 2.27 (s, 6H), 4.52 (s, 2H), 5.23(s, 2H), 7.09 (s, 2H), 7.51 (t, J=8.2 Hz, 1H), 7.76 (t, J=7.4 Hz, 1H), 8.17 (d, J=8.2 Hz, 1H), 8.18 (d, J=7.4 Hz, 1H); 13C NMR (68 MHz, CDCI3) d 16.4, 46.2, 70.1, 124.9, 128.2, 128.4, 129.5, 131.5, 133.5, 134.2, 134.7, 146.6, 155.6.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06657052B1 |
| Source dataset | uspto-grants-2003_12 |
| ORD ID | ord-7e0c37ee3db74feda47883a51d77462a |
| Source note | uspto-grants-2003_12 |