HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 66905406, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | HCID 86640271 | HCID 86640271 | — |
| Solvent | Thionyl Chloride | HCID 24386 | — |
| Product | HCID 66905406 | HCID 66905406 | 95% |
Reaction Steps
2-Azido-N-(4-chloro-phenyl)-4-fluoro-benzamide (2.7 g, 1 mmol) was dissolved at ambient temperature in thionyl chloride (18.2 ml) under an argon atmosphere. The reaction mixture was heated under reflux conditions for 14 h and brought to dryness under reduced pressure. The residue was taken up in ice water/saturated aqueous NaHCO3 solution 1/1 and CH2Cl2. The layers were separated and the aqueous layer was extracted one more time with CH2Cl2. The combined extracts were washed with ice water/brine 1/1 and dried over Na2SO4. The solvent was removed under reduced pressure to give the title compound (2.47 g, 8.8 mmol; 95%) as yellow solid. MS: m/e=280.9 [M+H+].
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08153663B2 |
| Source dataset | uspto-grants-2012_04 |
| ORD ID | ord-2dfece86d2734c7bba6c808665f01bb3 |
| Source note | uspto-grants-2012_04 |