4-Nitrobenzaldehyde → HCID 21249966、化合物

HRID 1531650ノート

反応式

HRID 1531650 の反応式
[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

参加物

6

反応物 2

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

生成物 1

HCID 21249966HCID 21249966、化合物収率 67%

試薬・触媒・溶媒 3

HCID 3007855Zincchloride触媒HCID 241Benzene溶媒HCID 8857Ethyl Acetate溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-2b89ce5f6ae94ad0a10ec36c02ddb558
出典データセット
uspto-grants-2001_03
特許番号
US06200970B1

反応ノート

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