HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86605971, compound → HCID 69520108, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86605971 | HCID 86605971 | — |
| Reactant | HCID 178461630 | HCID 178461630 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Solvent | Sodium chloride; water | HCID 57417360 | — |
| Product | HCID 69520108 | HCID 69520108 | — |
Reaction Steps
Fe(acac)3 (5 mg) followed by EtMgBr (0.73 mL, 1N in THF) is added to a solution of the amide obtained in Example 4 (129 mg) in 3 mL of THF and 0.3 mL of N-methylpyrrolidinone at room temperature under N2. The dark purple reaction mixture is stirred at room temperature for 50 min and then diluted with brine and extracted 3 times with EtOAc (10 mL). The combined extracts are dried over Na2SO4, filtered and concentrated under reduced pressure. The crude product is purified by preparative thin layer chromatography, developing 2 times with 25-1 CHCl3-MeOH (25-1) to afford the desired product. LC/MS: 422 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07253168B2 |
| Source dataset | uspto-grants-2007_08 |
| ORD ID | ord-321e1553291749a187f121f8ffdbd5c0 |
| Source note | uspto-grants-2007_08 |