HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Chloro-7-fluoroquinoline-3-carbaldehyde → 1-(2-Chloro-7-fluoroquinolin-3-yl)ethanol
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Chloro-7-fluoroquinoline-3-carbaldehyde | HCID 12099179 | — |
| Reactant | HCID 178418689 | HCID 178418689 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 1-(2-Chloro-7-fluoroquinolin-3-yl)ethanol | HCID 24276077 | — |
Reaction Steps
To a suspension of 2-chloro-7-fluoroquinoline-3-carbaldehyde (44.7 g, 213 mmol) in THF (600 mL) was treated with MeMgBr (78 mL, 1.1 eq) dropwise at −20° C. After overnight, the reaction was quenched with NH4Cl solution and extracted with Ether (300 mL and 100 mL). The organics were washed with water, brine, dried over Na2SO4, concentrated and recrystallized from EtOAc (100 mL) and hexane (1 L). A pale yellow solid was obtained (41 g, 85%). 1H NMR (400 MHz, CDCl3) δ ppm 8.41 (s, 1H), 7.87 (dd, J=8.0, 4.0 Hz, 1H), 7.67 (dd, J=8.0, 2.0 Hz, 1H), 7.38 (td, J=8.0, 2.0 Hz, 1H), 5.38 (q, J=4.0 Hz, 1H), 1.63 (d, J=4.0 Hz, 3H). Mass Spectrum (ESI) m/e=226 (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08901135B2 |
| Source dataset | uspto-grants-2014_12 |
| ORD ID | ord-cb6afc15cf1543ba932db58b25a3b429 |
| Source note | uspto-grants-2014_12 |