HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 70558051, compound → HCID 70558071, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 70558051 | HCID 70558051 | — |
| Reactant | HCID 178478100 | HCID 178478100 | — |
| Catalyst | Tetrakis(triphenylphosphine)palladium | HCID 11979704 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 70558071 | HCID 70558071 | — |
Reaction Conditions
| Temperature | 100 °C |
|---|
Reaction Steps
A suspension of the product of Example 10B (1.1 g, 3.0 mmol), IM (2,6-dichlorobenzyl)zinc(II) bromide in tetrahydrofuran (30 mL, 30 mmol) and tetrakis(triphenylphosphine) palladium(0) (347 mg, 0.3 mmol) in tetrahydrofuran (50 mL) was heated in a sealed tube at 100° C. under nitrogen for 16 hours. The cooled mixture was washed with saturated ammonium chloride solution (50 mL) and extracted with ethyl acetate (3×50 mL). The combined organic phase was dried over anhydrous sodium sulfate, filtered, concentrated and purified by flash chromatography on silica gel (200-300 mesh) eluting with 3/1 petroleum ether/ethyl acetate to give the title compound. MS: 476 (M+H+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09212192B2 |
| Source dataset | uspto-grants-2015_12 |
| ORD ID | ord-16e9ab28688648cd9a102973582101b8 |
| Source note | uspto-grants-2015_12 |