HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 178522672, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | HOAt | HCID 181649 | — |
| Reactant | HCID 86614808 | HCID 86614808 | — |
| Reactant | HCID 178509299 | HCID 178509299 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 178522672 | HCID 178522672 | — |
Reaction Steps
To a solution of the intermediate from step B (45 mg, 0.84 mmol) in DMF was added HOAt (17 mg, 0.126 mmol), DIEA (44 μL, 0.252 mmol), amino tetrazole (22 mg, 0.252 mmol) and EDC (24 mg, 0.126 mmol). The resulting solution was left stirring at room temperature for 18 hours. The reaction mixture was diluted with ethyl acetate (20 mL), and washed with 1N HCl. The organic layer was dried over anhydrous Na2SO4, filtered and concentrated in vacuo. The residue was purified on the Gilson reverse phase HPLC to give the title compound. 1H NMR (DMSO, 500 MHz): 8.04 (d, J=8.3 Hz, 2H), 7.82 (d, J=9.2 Hz, 2H), 7.74 (dd, J=6.9, 8.7 Hz, 2H), 7.64 (s, 1H), 7.38 (d, J=7.9 Hz, 2H), 5.85 (s, 2H). LC-MS: 2.56 min; (M+H)=603.1.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07649009B2 |
| Source dataset | uspto-grants-2010_01 |
| ORD ID | ord-142a146bd3f148aeaca510e7f451811b |
| Source note | uspto-grants-2010_01 |