Nitric Acid → Acetamide, N-(3-nitro(1,1'-biphenyl)-4-yl)-

HRID 859063

반응식

HRID 859063 반응식
[C:1]([NH:4][C:5]1[CH:10]=[CH:9][C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)=[CH:7][CH:6]=1)(=[O:3])[CH3:2].C(OC(=O)C)(=O)C.[N+:24]([O-])([OH:26])=[O:25]>O>[N+:24]([C:6]1[CH:7]=[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[CH:9]=[CH:10][C:5]=1[NH:4][C:1](=[O:3])[CH3:2])([O-:26])=[O:25]

참가 물질

5

반응물 3

HCID 944Nitric AcidHCID 7918Acetic AnhydrideHCID 19998N-Acetyl-4-aminobiphenyl

생성물 1

HCID 79364Acetamide, N-(3-nitro(1,1'-biphenyl)-4-yl)-

시약·촉매·용매 1

HCID 962Water용매

실험 절차

To a mixture of 4-acetamido-1,1′biphenyl (21.1 g, 0.1 mol) and 150 mL of acetic anhydride maintained between 8° C. and 13° C. is slowly added dropwise over 32 minutes 12.7 mL of 70% nitric acid. The reaction mixture is added to 600 mL of a mixture of water and ice and the resultant precipitate is collected by filtration. The filter cake is washed with water and the residue is recrystallized from methanol (800 mL) to give 23.6 g of the title compound as a yellow crystalline solid melting at 129–132° C.

후처리

  1. temperaturemaintained between 8° C. and 13° C.
  2. filtrationthe resultant precipitate is collected by filtration
  3. washThe filter cake is washed with water
  4. customthe residue is recrystallized from methanol (800 mL)

출처 및 근거

ORD 기록
ord-981f186ace28470a9cf664caae25ecc3
출처 데이터셋
uspto-grants-2006_12
특허 번호
US07148274B2

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