HuagongsheHuagongshe Chemistry Print Report · For research reference only
Cyanamide → HCID 86711639, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Cyanamide | HCID 9864 | — |
| Reactant | Sodium Thiosulfate | HCID 24477 | — |
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | HCID 86711640 | HCID 86711640 | — |
| Solvent | Methanol | HCID 887 | — |
| Product | HCID 86711639 | HCID 86711639 | — |
Reaction Steps
N-Bromosuccinimide (63 mg, 0.35 mmol) is added to a mixture of 1-isopropyl-6-methyl-4-oxo-5-(3-trifluoromethyl-phenyl)-1,4-dihydro-pyridine-3-carboxylic acid 3-methyl-4-methylsulfanyl-benzylamide (preparation 66c, 115 mg, 0.24 mmol), cyanamide (14 mg, 0.33 mmol) and potassium tert-butoxide (32 mg, 0.29 mmol) in methanol (1.1 mL). After 20 min saturated aqueous sodium thiosulfate solution is added, and the mixture is extracted twice with dichloromethane. The combined organic layers is dried over Na2SO4 and concentrated under reduced pressure. The residue is directly used in the next step without further purification. Yield: 99 mg (80% of theory); ESI mass spectrum: [M+H]+=529; r.t. HPLC: 0.58 min (X012_S01).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09346794B1 |
| Source dataset | uspto-grants-2016_05 |
| ORD ID | ord-b54b09916df844278e25ecc839a0e625 |
| Source note | uspto-grants-2016_05 |