HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethyl diazoacetate → HCID 178438678, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethyl diazoacetate | HCID 12192 | — |
| Reactant | HCID 178438589 | HCID 178438589 | — |
| Catalyst | Acetic acid, rhodium(2+) salt | HCID 21674 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 178438678 | HCID 178438678 | — |
Reaction Steps
To a mixture of 4′-{[4-(trans-4-hydroxycyclohexyl)-5-oxo-7-propyl-4,5-dihydro[1,2,3]triazolo[1,5-a]pyrimidin-6-yl]methyl}biphenyl-2-carbonitrile (470 mg), rhodium(II) acetate (dimer) (22 mg) and methylene chloride (10 mL) was added dropwise ethyl diazoacetate (137 mg) under an argon atmosphere, and the mixture was stirred at room temperature for 3 days. The reaction mixture was washed with water and then with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel chromatography [eluent: hexane/ethyl acetate=70/30→20/80 (volume ratio)] to give the title compound as a colorless amorphous compound (203 mg, 37%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08592431B2 |
| Source dataset | uspto-grants-2013_11 |
| ORD ID | ord-6baa909325ef48cc9ee21bbfbe4ca982 |
| Source note | uspto-grants-2013_11 |