반응 #3216

반응 방정식

water

sodium hydroxide

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

→

title compound

수율 80.2%

Methyl 2-amino-4-iodobenzoate

수율 80.2%

용매

methanol

반응 조건

후처리

1. 1
   온도the resulting solution was cooled
2. 2
   추출extracted with ethyl acetate
3. 3
   세척The combined extracts were washed once with dilute sodium hydroxide
4. 4
   건조dried (MgSO4)
5. 5
   여과filtered
6. 6
   농축concentrated

실험 절차

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).

출처