HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 59390004, compound → HCID 68459644, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 59390004 | HCID 59390004 | — |
| Reactant | HCID 178418368 | HCID 178418368 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Solvent | N-methyl-2-pyrrolidone | HCID 13387 | — |
| Product | HCID 68459644 | HCID 68459644 | — |
Reaction Steps
The product from Example 12b (1.0 g, 4.84 mmol) was treated with 2.0 M isobutylmagnesium chloride (2.90 mL, 5.81 mmol) in 30 mL THF and 3 mL NMP at room temperature under a N2 atmosphere. Added Fe(acac)3 (85 mg, 0.242 mmol) and stirred at room temperature for 18 h. During the course of the reaction two additional charges of Grignard reagent and catalyst were added. The reaction was quenched by pouring into 5% acetic acid and extracting with ether. Dried over Na2SO4, filtered and concentrated under vacuum giving the title compound that was purified by silica gel column chromatography eluting with 10% EtOAc/hexane to give (620 mg, 56%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08338605B2 |
| Source dataset | uspto-grants-2012_12 |
| ORD ID | ord-c6ff0304825b4a3193124dc06ab68d04 |
| Source note | uspto-grants-2012_12 |