반응 #214624

반응 방정식

acetic anhydride

1,4-benzodioxane-5-carboxylic acid

nitric acid

→

6-nitro-1,4-benzodioxane-5-carboxylic acid

용매

acetic acid

acetic acid

반응 조건

후처리

1. 1
   기타provided with an agitator
2. 2
   온도cooled to 5° C
3. 3
   기타The precipitate was dried off
4. 4
   세척washed with 600 ml of acetic acid
5. 5
   건조with water and dried at 40° C
6. 6
   기타700 g of 7-nitro-1,4-benzodioxane-5-carboxylic acid were collected
7. 7
   workup.ADDITIONwere diluted with 25 liters of water
8. 8
   기타the obtained precipitate was dried off
9. 9
   세척washed with water
10. 10
    기타dried

실험 절차

1,600 ml of acetic acid, 1,600 ml of acetic anhydride, and 1000 g of 1,4-benzodioxane-5-carboxylic acid were introduced in a 6-liter balloon flask provided with an agitator and a thermometer. The mixture was heated to 40° C. and a solution of 400 ml of nitric acid in 400 ml of acetic acid was added. After the introduction, the mixture was stirred at 40°-45° C. for two hours and then cooled to 5° C. The precipitate was dried off, washed with 600 ml of acetic acid and then with water and dried at 40° C. 700 g of 7-nitro-1,4-benzodioxane-5-carboxylic acid were collected, the structure of which was confirmed by nuclear magnetic resonance (M.P.: 246° C.) The mother liquors were diluted with 25 liters of water and the obtained precipitate was dried off, washed with water and dried. 6-nitro-1,4-benzodioxane-5-carboxylic acid was obtained (M.P.: 188° C.).

출처