HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tetrahydrofuran → HCID 11256967, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tetrahydrofuran | HCID 8028 | — |
| Reactant | 2-Iodopyridine | HCID 221126 | — |
| Reactant | HCID 67024193 | HCID 67024193 | — |
| Reactant | HCID 178478990 | HCID 178478990 | — |
| Product | HCID 11256967 | HCID 11256967 | 33% |
Reaction Steps
Cyclohexylmagnesium chloride (5 mL, 2.0 M in Et2O) was added dropwise to the solution of 2-iodopyridine (1.03 g, 5 mmol) in THF (15 mL) at −20° C. The mixture was stirred at this temperature for 20 min before 3-(5-Amino-4-cyano-pyrazol-1-yl)-N-cyclopropyl-4-methyl-benzamide (140 mg, 0.5 mmol) was added, then stirred at room temperature over night. The reaction was quenched by the addition of K2CO3 aqueous solution, then the mixture was extracted with EtOAc and the organic layers washed with water and brine. Purification by column chromatography on silica gel eluted with EtOAc provided the product as a white solid (60 mg, 33%). HPLC (4 minute 10-90 gradient) tR 2.09 min; MS m/z 362.20 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08410160B2 |
| Source dataset | uspto-grants-2013_04 |
| ORD ID | ord-67fd819ffaf94242948259cd332ecebd |
| Source note | uspto-grants-2013_04 |