HuagongsheHuagongshe Chemistry Print Report · For research reference only
(Methoxycarbonylsulfamoyl)triethylammonium hydroxide → US9290457, Example 8
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | (Methoxycarbonylsulfamoyl)triethylammonium hydroxide | HCID 11032497 | — |
| Reactant | 2-[5-Acetyl-3,6-dimethyl-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2,3,4-tetrahydro-pyrimidin-4-yl]-5-cyano-benzoic acid acetyl hydrazide | HCID 118691673 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | US9290457, Example 8 | HCID 118691694 | — |
Reaction Steps
2-[5-Acetyl-3,6-dimethyl-2-oxo-1-(3-trifluoromethyl-phenyl)-1,2,3,4-tetrahydro-pyrimidin-4-yl]-5-cyano-benzoic acid acetyl hydrazide (intermediate 13) (15 mg, 0.03 mmol) is suspended in dichloromethane (1 mL) and (methoxycarbonylsulfamoyl)triethyl-ammonium hydroxide (Burgess reagent)(17.4 mg, 0.07 mmol) is added. The mixture is stirred at room temperature for 3 days. The solvent is removed under reduced pressure and purification is performed by reversed phase HPLC. Yield: 6.4 mg; ESI mass spectrum [M+H]+=496; Retention time HPLC: 1.04 min (HPLC method Z018_S04).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09290457B2 |
| Source dataset | uspto-grants-2016_03 |
| ORD ID | ord-7654b0ec4a364ab8ad060ed56a5b15cb |
| Source note | uspto-grants-2016_03 |