Sulfuric Acid → 3-Oxo-1,3-dihydro-2,1-benzoxazole-5,7-dicarboxylic acid

HRID 2049909

반응식

HRID 2049909 반응식
[N+:1]([C:4]1[C:12]([C:13]([OH:15])=[O:14])=[CH:11][C:10]([C:16]([OH:18])=[O:17])=[CH:9][C:5]=1[C:6]([OH:8])=[O:7])([O-])=O.[Mn]([O-])(=O)(=O)=O.[K+].[N+](C1C(C)=CC(C)=CC=1C)([O-])=O.S(=O)(=O)(O)O>[Zn].C(OCC)(=O)C.O>[C:16]([C:10]1[CH:9]=[C:5]([C:6]([OH:8])=[O:7])[C:4]2[NH:1][O:14][C:13](=[O:15])[C:12]=2[CH:11]=1)([OH:18])=[O:17]

참가 물질

8

반응물 4

HCID 1118Sulfuric AcidHCID 690512-NitromesityleneHCID 516875Potassium PermanganateHCID 32590422-nitrobenzene-1,3,5-tricarboxylic Acid

생성물 1

HCID 134113503-Oxo-1,3-dihydro-2,1-benzoxazole-5,7-dicarboxylic acid

시약·촉매·용매 3

HCID 23994Zinc촉매HCID 962Water용매HCID 8857Ethyl Acetate용매

실험 절차

To a stirred solution of 12.8 g. of nitrotrimesic acid (prepared by alkaline potassium permanganate oxidation of nitromesitylene) in 200 ml. of water containing 30 g. of sulfuric acid are added 6.5 g. of zinc dust in portions at such a rate so as to maintain a temperature of about 25° C. After the addition, the mixture is stirred for an additional 1 hr. After this time, 200 ml. of ethyl acetate are added and the mixture is rapidly stirred for 15 min. The reaction is then filtered by suction through a pad of filter aid. The organic layer is separated, dried and concentrated under reduced pressure, leaving 9.6 g. of crude product which is used directly in the next step. ##STR15##

후처리

  1. additionAfter the addition
  2. stirringthe mixture is rapidly stirred for 15 min
  3. filtrationThe reaction is then filtered by suction through a pad of filter aid
  4. customThe organic layer is separated
  5. customdried
  6. concentrationconcentrated under reduced pressure
  7. customleaving 9.6 g

출처 및 근거

ORD 기록
ord-ceda8a4d3d764a798064ec8dccea5e95
출처 데이터셋
uspto-grants-1980_04
특허 번호
US04199354

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