Dimethylformamide → 3-Azaisatoic anhydride

HRID 268328노트

반응식

HRID 268328 반응식
C([C:4]1[N:12]=[CH:11][CH:10]=[CH:9][C:5]=1[C:6]([OH:8])=[O:7])(=O)N.C[N:14](C)[CH:15]=[O:16].C([O-])(=O)C.C([O-])(=O)C.C([O-])(=O)C.C([O-])(=O)C.[Pb+4]>O>[C:5]12[C:4](=[N:12][CH:11]=[CH:10][CH:9]=1)[NH:14][C:15](=[O:16])[O:8][C:6]2=[O:7]

참가 물질

5

반응물 3

HCID 6228DimethylformamideHCID 2588102-Carbamoylpyridine-3-carboxylic acidHCID 178418268HCID 178418268, 화합물

생성물 1

HCID 109865823-Azaisatoic anhydride

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A 100 ml. flask was charged with 2.0 g. 2-carbamylnicotinic acid* suspended in 20 ml. dimethylformamide. A 5.5 g. portion of lead tetra-acetate was added to the suspension, and the mixture was stirred at 50°-60° for 1 hour. The reaction mixture was poured into 20 ml. water; solids were separated by filtration, and 3-azaisatoic anhydride was recrystallized from dioxane, and dried in vacuo for 2 hours. The final yield of 3-azaisatoic anhydride amounted to 1.48 g., melting point 217°-219°, and represented 75 percent of theory. The structure was confirmed by elemental analysis and infrared spectroscopy.

후처리

  1. additionflask was charged with 2.0 g
  2. additionThe reaction mixture was poured into 20 ml
  3. customsolids were separated by filtration, and 3-azaisatoic anhydride
  4. customwas recrystallized from dioxane
  5. customdried in vacuo for 2 hours

출처 및 근거

ORD 기록
ord-de8ee2ee69854ba2a225a1fc50506a08
출처 데이터셋
uspto-grants-1976_03
특허 번호
US03947442

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