Acetic Acid → 2,2-dimethyl-5,6-dinitro-1,3-benzodioxole

HRID 2248107노트

반응식

HRID 2248107 반응식
[N+:1]([O-:4])([OH:3])=O.C(O)(=O)C.[CH3:9][C:10]1([CH3:22])[O:14][C:13]2[CH:15]=[CH:16][C:17]([N+:19]([O-:21])=[O:20])=[CH:18][C:12]=2[O:11]1>O>[CH3:9][C:10]1([CH3:22])[O:11][C:12]2[CH:18]=[C:17]([N+:19]([O-:21])=[O:20])[C:16]([N+:1]([O-:4])=[O:3])=[CH:15][C:13]=2[O:14]1

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 944Nitric AcidHCID 2330662,2-Dimethyl-5-nitro-1,3-benzodioxole

생성물 1

HCID 50472752,2-dimethyl-5,6-dinitro-1,3-benzodioxole수율 82%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A solution of 90% (fuming) nitric acid (22 ml) and glacial acetic acid (11 ml) cooled at 12° C. was treated in portions with solid compound from Example 3B (5.4 g, 27.7 mmoles) so as to maintain the temperature of <17° C. After the addition, stirring was continued for 15 minutes, when the internal temperature began to fall. The mixture was diluted to 100 ml with water, the yellow solid filtered, washed with water, taken up in CH2Cl2, dried (Na2SO4) and evaporated to give 5.43 g (82%) of pure title compound.

후처리

  1. temperatureto maintain the temperature of <17° C
  2. additionAfter the addition
  3. filtrationthe yellow solid filtered
  4. washwashed with water
  5. dry with materialdried (Na2SO4)
  6. customevaporated

출처 및 근거

ORD 기록
ord-a29cdd118e834e90807861c774570d23
출처 데이터셋
uspto-grants-1991_08
특허 번호
US05037983

반응 노트

불러오는 중…