Nitric Acid → 1-(5-(Benzyloxy)-2-hydroxy-3-nitrophenyl)ethanone

HRID 1662953노트

반응식

HRID 1662953 반응식
[N+:1]([O-:4])(O)=[O:2].[CH2:5]([O:12][C:13]1[CH:14]=[CH:15][C:16]([OH:22])=[C:17]([C:19](=[O:21])[CH3:20])[CH:18]=1)[C:6]1[CH:11]=[CH:10][CH:9]=[CH:8][CH:7]=1>C(O)(=O)C>[CH2:5]([O:12][C:13]1[CH:14]=[C:15]([N+:1]([O-:4])=[O:2])[C:16]([OH:22])=[C:17]([C:19](=[O:21])[CH3:20])[CH:18]=1)[C:6]1[CH:7]=[CH:8][CH:9]=[CH:10][CH:11]=1

참가 물질

4

반응물 2

HCID 944Nitric AcidHCID 128709281-[5-(Benzyloxy)-2-hydroxyphenyl]ethan-1-one

생성물 1

HCID 210728231-(5-(Benzyloxy)-2-hydroxy-3-nitrophenyl)ethanone

시약·촉매·용매 1

HCID 176Acetic Acid용매

실험 절차

18 mL fuming nitric acid are added dropwise to a solution of 81.5 g (0.34 mol) 1-(5-benzyloxy-2-hydroxyphenyl)-ethanone in 700 mL acetic acid while cooling with the ice bath, so that the temperature does not exceed 20° C. Then the reaction mixture is stirred for two hours at ambient temperature, poured onto ice water and filtered. The product is recrystallized from isopropanol, suction filtered and washed with isopropanol and diisopropylether. Yield: 69.6 g (72%); mass spectroscopy [M+H]+=288.

후처리

  1. customdoes not exceed 20° C
  2. additionpoured onto ice water
  3. filtrationfiltered
  4. customThe product is recrystallized from isopropanol, suction
  5. filtrationfiltered
  6. washwashed with isopropanol and diisopropylether

출처 및 근거

ORD 기록
ord-a1273b85820b445d9832cd1d392b8c87
출처 데이터셋
uspto-grants-2011_10
특허 번호
US08034809B2

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