Acetic Acid → 2,2-Dimethyl-5-nitro-1,3-benzodioxole

HRID 2248106노트

반응식

HRID 2248106 반응식
[N+:1]([O-:4])(O)=[O:2].C(O)(=O)C.[CH3:9][C:10]1([CH3:19])[O:14][C:13]2[CH:15]=[CH:16][CH:17]=[CH:18][C:12]=2[O:11]1>O>[CH3:9][C:10]1([CH3:19])[O:11][C:12]2[CH:18]=[CH:17][C:16]([N+:1]([O-:4])=[O:2])=[CH:15][C:13]=2[O:14]1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 944Nitric AcidHCID 2858692,2-dimethyl-2H-1,3-benzodioxole

생성물 1

HCID 2330662,2-Dimethyl-5-nitro-1,3-benzodioxole

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 70% (conc.) nitric acid (20 ml) and glacial acetic acid (10 ml) cooled at 12° C. was treated by drops with 5 g (33.3 mmole) of the compound of Example 3A at a rate to maintain the temperature at 15°-20° C. Stirring was continued for 15 minutes after addition, then the brown slurry was diluted to 100 ml with water and filtered. The solid was washed with water, taken up in CH2Cl2, dried (Na2SO4) and evaporated to 5.40 g (83%) of pure yellow mononitro title compound.

후처리

  1. temperatureto maintain the temperature at 15°-20° C
  2. additionafter addition
  3. filtrationfiltered
  4. washThe solid was washed with water
  5. dry with materialdried (Na2SO4)
  6. customevaporated to 5.40 g (83%) of pure yellow mononitro title compound

출처 및 근거

ORD 기록
ord-59ccbc6a7b29438d8b15da99e1c42378
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05037983

반응 노트

불러오는 중…