4-Nitrobenzaldehyde → HCID 21249966, 화합물

HRID 1531650노트

반응식

HRID 1531650 반응식
[Br:1][C:2]1[CH:3]=[C:4]([CH2:10][CH2:11][OH:12])[CH:5]=[CH:6][C:7]=1[O:8][CH3:9].[N+:13]([C:16]1[CH:23]=[CH:22][C:19]([CH:20]=O)=[CH:18][CH:17]=1)([O-:15])=[O:14]>C1C=CC=CC=1.C(OCC)(=O)C.[Cl-].[Zn+2].[Cl-]>[Br:1][C:2]1[CH:3]=[C:4]2[C:5](=[CH:6][C:7]=1[O:8][CH3:9])[CH:20]([C:19]1[CH:22]=[CH:23][C:16]([N+:13]([O-:15])=[O:14])=[CH:17][CH:18]=1)[O:12][CH2:11][CH2:10]2

참가 물질

6

반응물 2

HCID 5414-NitrobenzaldehydeHCID 230022542-(3-Bromo-4-methoxyphenyl)ethanol

생성물 1

HCID 21249966HCID 21249966, 화합물수율 67%

시약·촉매·용매 3

HCID 3007855Zincchloride촉매HCID 241Benzene용매HCID 8857Ethyl Acetate용매

실험 절차

Hydrogen chloride gas that is dried for 5 hours is introduced into a suspension of 7.50 g (32.4 mmol) of 2-(3-bromo-4-methoxy-phenyl)-ethanol, 4.90 g (32.4 mmol) of 4-nitro-benzaldehyde and 4.39 g (32.4 mmol) of freshly melted zinc chloride in anhydrous benzene (96 ml). The reaction mixture is then diluted with ethyl acetate and washed neutral with water. After drying and concentration by evaporation, the solid residue is recrystallized from ethyl acetate (25 ml). 7.91 g (67%) of 6-bromo-7-methoxy-l-(4-nitrophenyl)-isochroman, melting point 144-147° C., is obtained.

후처리

  1. dry with materialHydrogen chloride gas that is dried for 5 hours
  2. washwashed neutral with water
  3. customAfter drying
  4. concentrationconcentration
  5. customby evaporation
  6. customthe solid residue is recrystallized from ethyl acetate (25 ml)

출처 및 근거

ORD 기록
ord-2b89ce5f6ae94ad0a10ec36c02ddb558
출처 데이터셋
uspto-grants-2001_03
특허 번호
US06200970B1

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