HuagongsheHuagongshe Chemistry Print Report · For research reference only
1,2-Dichloroethane → HCID 117628496, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 1,2-Dichloroethane | HCID 11 | — |
| Reactant | 2,2,2-Trifluoroethylamine hydrochloride | HCID 9772 | — |
| Reactant | 1-Hydroxybenzotriazole | HCID 75771 | — |
| Reactant | HCID 89486950 | HCID 89486950 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 117628496 | HCID 117628496 | — |
Reaction Steps
(Cis)-2-[(6-chloropyridazin-4-yl)amino]cyclohexanecarboxylic acid I-22b (2.2 g, 8.60 mmol), HOBT (2.64 g, 17.21 mmol), EDC (3.30 g, 17.21 mmol) and trifluoroethyl amine hydrochloride (2.332 g, 17.21 mmol) were added to DCM (30.0 ml) followed by the addition of TEA (6.00 ml, 43.0 mmol). The slurry was allowed to stir at RT for 17 hr. The reaction was diluted with dichloromethane washed with sat. sodium bicarb., brine dried with sodium sulfate and concentrated to an oil. Purification on Biotage Normal Phase system (DCMeOH, 0-8% B) afforded the product I-22 as a solid. (1.56 g, 51.2%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09096598B2 |
| Source dataset | uspto-grants-2015_08 |
| ORD ID | ord-249cfcbdc49142a28defca3b3395259d |
| Source note | uspto-grants-2015_08 |