Sodium Iodide → HCID 46919443, Verbindung

To a solution of chloromethyl 4-fluorobenzoate (3.0g, 15.9 mmol) in 50 mL of dry acetone, NaI (4.8 g, 31.8 mmol) was added and the mixture was stirred overnight. The solvent was removed and Et2O (150 mL) was added to the solid residues and the mixture was stirred for 10 min. After filtration the filtrate was washed with 5% NaHSO3 (aq) (2×25 mL) followed by brine. The organic solution was concentrated by rotary evaporation and purified by silica gel chromatography to give a light yellow oil. Yield 3.7 g (85%). 1H NMR (300 MHz, CDCl3): δ 6.16 (s, 2H), 7.17 (m, 2H), 8.08 (m, 2H).

1. customThe solvent was removed
2. additionEt2O (150 mL) was added to the solid residues
3. stirringthe mixture was stirred for 10 min
4. filtrationAfter filtration the filtrate
5. washwas washed with 5% NaHSO3 (aq) (2×25 mL)
6. concentrationThe organic solution was concentrated by rotary evaporation
7. custompurified by silica gel chromatography
8. customto give a light yellow oil

ORD-Eintrag

ord-3a7da02939a042cb873473416ffb7bfe

Quelldatensatz

uspto-grants-2014_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08841257B2