HuagongsheHuagongshe Chemistry Print Report · For research reference only
Dichloromethane → HCID 178463344, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Trifluoroacetic acid methylene chloride | HCID 21863450 | — |
| Reactant | HCID 178463345 | HCID 178463345 | — |
| Solvent | Water | HCID 962 | — |
| Product | HCID 178463344 | HCID 178463344 | 488.2% |
Reaction Steps
(S)-tert-Butyl 4-(trans-4-(4-chloro-3-(ethylamino)phenylsulfonamido)cyclo-hexanecarbonyl)-3-phenylpiperazine-1-carboxylate (Example 1, 77 mg, 0.127 mmol) was stirred in 20% v/v TFA/DCM overnight. The reaction was dilutee with DCM and water and the pH was adjusted to 13 with 1N NaOH. The layers were separated, and the organic layer was concentrated and chromatographed on reverse phase Phenomenex Gemini Axia C18 30×100 mm column using a gradient of 15-100% AcCN in water containing 5 mM ammonium hydroxide. The product was lyophilized to yield the title compound (31.5 mg, 0.62 mmol). MS MH+ 505.4.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08394858B2 |
| Source dataset | uspto-grants-2013_03 |
| ORD ID | ord-ae3d8e396e9c4ebe999c37e02be6e859 |
| Source note | uspto-grants-2013_03 |