HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 69268257, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | HOAt | HCID 181649 | — |
| Reactant | HCID 11307452 | HCID 11307452 | — |
| Reactant | (4-Bromo-2-fluorophenyl)methanaminium chloride | HCID 45075641 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 69268257 | HCID 69268257 | — |
Reaction Steps
Triethylamine (1.036 g, 10.24 mmol) was added to a stirred solution of the compound of reference Example 3 (2.556 g, 10.24 mmol), (4-bromo-2-fluorophenyl)methanaminium chloride (2.463 g, 10.24 mmol), EDC (1.963 g, 10.24 mmol), and HOAT (0.418 g, 3.072 mmol) in CH2Cl2 (25 mL). After 1 h, the reaction was diluted with water and extracted with ethyl acetate. The organic extract was washed with water, dried over sodium sulfate, filtered and concentrated under reduced pressure to yield a yellow solid. This solid was purified by silica gel chromatography, eluting with 5% methanol/CH2Cl2 to yield N-(1-{[(4-bromo-2-fluorobenzyl)amino]carbonyl}cyclopropyl)pyrimidine-5-carboxamide as a white solid. Low resolution MS: (M+H+)=393.03.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07332499B2 |
| Source dataset | uspto-grants-2008_02 |
| ORD ID | ord-242e30932d214545b494277a7299ca75 |
| Source note | uspto-grants-2008_02 |