Reaktion #745518

Reaktionsgleichung

3-tert-Butoxy-5-fluoro-phenyl-amine

Thiophosgene

K2CO3

→

dichloromethane iso-hexane

title compound

1-tert-Butoxy-3-fluoro-5-isothiocyanatobenzene

Lösungsmittel

CHCl3

CHCl3

H2O

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe organics are separated
2. 2
   Waschenwashed with water (3×), brine (1×)
3. 3
   Trocknendried over MgSO4
4. 4
   Filtrationfiltered
5. 5
   Sonstigethe solvent removed in vacuo

Vorschrift

Thiophosgene (33.6 g) in CHCl3 (250 ml) and K2CO3 (64.7 g) in H2O (450 ml) are added, separately and simultaneously, drop wise to a solution of 3-tert-Butoxy-5-fluoro-phenyl-amine (42.9 g) in CHCl3 (350 ml) at 0° C. The reaction mixture is warmed to room temperature over night. The organics are separated and washed with water (3×), brine (1×), dried over MgSO4, filtered and the solvent removed in vacuo. The title compound is obtained by flash column chromatography (silica, eluent dichloromethane/iso-hexane 1:3). 1H nmr (CDCl3, 400 MHz); 6.70 (m, 3H), 1.40 (s, 9H).

Quelle