HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-methyl-2-pyrrolidone → 1-(2-Chloro-4,5-difluorobenzoyl)-3-(5-amino-2-methoxyphenyl)urea
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Reactant | 1-(2-Chloro4,5-difluorobenzoyl)-3-(2-methoxy-5-nitrophenyl)urea | HCID 11668152 | — |
| Reactant | Tin dichloride dihydrate | HCID 43835034 | — |
| Solvent | Ethylacetate methanol | HCID 21584119 | — |
| Product | 1-(2-Chloro-4,5-difluorobenzoyl)-3-(5-amino-2-methoxyphenyl)urea | HCID 11566579 | 67% |
Reaction Steps
5.8 g (25.9 mmol) of tin dichloride hydrate were added to 2.0 g (5.2 mmol) of 1-(2-chloro-4,5-difluorobenzoyl)-3-(2-methoxy-5-nitrophenyl)urea in 20 ml of ethyl acetate/methanol mixture at 70° C. After 1 hour, 30 ml of N-methyl-2-pyrrolidinone were added, and the mixture was stirred for a further 2 hours. After cooling, the reaction mixture was made basic and the resulting precipitate was filtered off with suction. The phases were separated. The organic phase was then washed three times with water, dried and concentrated under high vacuum. 1.2 g (67%) of the desired product were obtained.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08247452B2 |
| Source dataset | uspto-grants-2012_08 |
| ORD ID | ord-b620a01271774162a39ac485a129fc22 |
| Source note | uspto-grants-2012_08 |