HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 89714813, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 2,4-Difluoroaniline | HCID 9709 | — |
| Reactant | Triphosgene | HCID 94429 | — |
| Reactant | HCID 89714581 | HCID 89714581 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 89714813 | HCID 89714813 | 84.2% |
Reaction Steps
To a solution of 350.35 mg (1.18 mmol) of triphosgene in 6 ml of DCM is added in a single portion a suspension of 500 mg (1.18 mmol) of 4-(4-aminophenyl)-6-ethyl-8,8-dimethyl-2-(8-oxa-3-azabicyclo[3.2.1]oct-3-yl)-7,8-dihydro-6H-9-oxa-1,3,6-triazabenzocyclohepten-5-one and 987.33 μl (7.08 mmol) of triethylamine in 6 ml of DCM. The resulting mixture is stirred for 20 minutes at room temperature. 607.12 μl (5.90 mmol) of 2,4-difluoroaniline are added. The precipitate obtained is filtered off, rinsed twice with MeOH and dried under reduced pressure to give 575 mg of 1-(2,4-difluorophenyl)-3-{4-[6-ethyl-8,8-dimethyl-2-(8-oxa-3-azabicyclo[3.2.1]oct-3-yl)-5-oxo-5,6,7,8-tetrahydro-9-oxa-1,3,6-triazabenzocyclohepten-4-yl]phenyl}urea.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09120812B2 |
| Source dataset | uspto-grants-2015_09 |
| ORD ID | ord-509da162a0cf4e16959b9339635aea3a |
| Source note | uspto-grants-2015_09 |