Acetic Acid → 2-Methylfuran-3-carboxamide

HRID 1416549노트

반응식

HRID 1416549 반응식
CN(C)N.ClC1C=CC([NH:12][C:13]([C:15]2[CH:19]=[CH:18][O:17][C:16]=2[CH3:20])=[O:14])=CC=1C=O.C(O)(=O)C>CO>[CH3:20][C:16]1[O:17][CH:18]=[CH:19][C:15]=1[C:13]([NH2:12])=[O:14]

참가 물질

5

반응물 3

HCID 176Acetic AcidHCID 59761,1-DimethylhydrazineHCID 54027287N-(4-chloro-3-formylphenyl)-2-methyl-3-furancarboxamide

생성물 1

HCID 107729742-Methylfuran-3-carboxamide

시약·촉매·용매 1

HCID 887Methanol용매2회

실험 절차

To the solution of 1,1-dimethylhydrazine (0.6 mL) in methanol (15 mL) was added, in portions, a suspension of N-(4-chloro-3-formylphenyl)-2-methyl-3-furancarboxamide (2 g) in methanol (30 mL) at such a rate that the temperature of the solution was maintained at -5° C. to 0° C. The resultant mixture was stirred overnight at ambient temperature. Acetic acid (0.1 mL) was then added to the reaction mixture which was then refluxed for 30 minutes, solvent was evaporated and the reaction mixture was poured into water and extracted with ethyl acetate. The organic layer was washed with water, dried (MgSO4) filtered and evaporated to produce N-[4-chloro-3-[dimethylhydrazono)methyl]phenyl]-2-methyl 3-furancarboxamide as a white solid, m.p. 109-111° C.

후처리

  1. temperaturewas maintained at -5° C. to 0° C
  2. temperaturewas then refluxed for 30 minutes
  3. customsolvent was evaporated
  4. additionthe reaction mixture was poured into water
  5. extractionextracted with ethyl acetate
  6. washThe organic layer was washed with water
  7. dry with materialdried (MgSO4)
  8. filtrationfiltered
  9. customevaporated

출처 및 근거

ORD 기록
ord-07a31af92a9948bb852ddb65ac2543d9
출처 데이터셋
uspto-grants-1999_06
특허 번호
US05914351

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