HuagongsheHuagongshe Chemistry Print Report · For research reference only
Thionyl Chloride → HCID 21913840, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 21914017 | HCID 21914017 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 21913840 | HCID 21913840 | 91.9% |
Reaction Steps
Thionyl chloride (3.14 mL, 43 mmol) was added over a period of 5 minutes to a chilled (0° C.) solution of 4-[(2,3-dimethyl-5-nitro-6-phenoxypyridin-4-yl)amino]butan-1-ol (12.95 g, 39.08 mmol) in dichloromethane (130 mL). The reaction was allowed to warm to ambient temperature and was stirred overnight under a nitrogen atmosphere. The reaction mixture was diluted with dichloromethane (130 mL), washed sequentially with saturated aqueous sodium bicarbonate (2×65 mL), water (80 mL) and brine (100 mL), dried over magnesium sulfate, filtered and then concentrated under reduced pressure to provide 12.57 g of N-(4-chlorobutyl)-2,3-dimethyl-5-nitro-6-phenoxypyridin-4-amine as a yellow solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07220758B2 |
| Source dataset | uspto-grants-2007_05 |
| ORD ID | ord-d74212e1952447c1a932c9db3ff746c9 |
| Source note | uspto-grants-2007_05 |