Reaktion #3216

Reaktionsgleichung

water

sodium hydroxide

7-iodo-2H-3,1-benzoxazine-2,4(1H)-dione

→

title compound

Ausbeute 80.2%

Methyl 2-amino-4-iodobenzoate

Ausbeute 80.2%

Lösungsmittel

methanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe resulting solution was cooled
2. 2
   Extraktionextracted with ethyl acetate
3. 3
   WaschenThe combined extracts were washed once with dilute sodium hydroxide
4. 4
   Trocknendried (MgSO4)
5. 5
   Filtrationfiltered
6. 6
   Einengenconcentrated

Vorschrift

To a stirred solution of sodium hydroxide (0.048 g, 1.2 mM) in methanol (4.5 mL) was added 7-iodo-2H-3,1-benzoxazine-2,4(1H)-dione (2.6 g, 9.0 mM). The mixture was heated at 60° C. for 7 hr and the resulting solution was cooled, poured into water and extracted with ethyl acetate. The combined extracts were washed once with dilute sodium hydroxide, dried (MgSO4), filtered and concentrated to leave the title compound (2.0 g, 80%) as a brown oil which slowly crystallized; MS(CI): 278 (M+H).

Quelle