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Benzyl Bromide → 2-(Benzyloxy)-1-bromo-3-nitrobenzene

HRID 1055684
ノート
印刷プレビュー

反応式

HRID 1055684 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([N+:8]([O-:10])=[O:9])[C:3]=1[OH:11].[CH2:12](Br)[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1.C(=O)([O-])[O-].[K+].[K+]>C(#N)C.C(OCC)(=O)C>[CH2:12]([O:11][C:3]1[C:4]([N+:8]([O-:10])=[O:9])=[CH:5][CH:6]=[CH:7][C:2]=1[Br:1])[C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 135454532-Bromo-6-nitrophenol

生成物 1

HCID 218735142-(Benzyloxy)-1-bromo-3-nitrobenzene

試薬・触媒・溶媒 2

HCID 6342Acetonitrile溶媒HCID 8857Ethyl Acetate溶媒

実験手順

A mixture of 5.22 g (23.9 mmol) of 2-bromo-6-nitrophenol, 3.0 ml (25.1 mmol) of benzyl bromide and 3.64 g (26.3 mmol) of potassium carbonate in 50 ml of acetonitrile was heated under reflux for 2 h. After cooling to RT, the solid was filtered off and the filtrate was freed from the solvent on a rotary evaporator. The residue obtained was dissolved in ethyl acetate and washed successively with water and saturated sodium chloride solution. After drying over anhydrous magnesium sulphate, the mixture was filtered and the filtrate was concentrated on a rotary evaporator. The residue that remained was dried under high vacuum. This gave 7.53 g (99% of theory) of the title compound.

後処理

  1. temperaturewas heated
  2. temperatureunder reflux for 2 h
  3. filtrationthe solid was filtered off
  4. customthe filtrate was freed from the solvent on a rotary evaporator
  5. customThe residue obtained
  6. washwashed successively with water and saturated sodium chloride solution
  7. dry with materialAfter drying over anhydrous magnesium sulphate
  8. filtrationthe mixture was filtered
  9. concentrationthe filtrate was concentrated on a rotary evaporator
  10. customThe residue that remained was dried under high vacuum

出典と根拠

ORDレコード
ord-0573ad9fc49d4c0a9f10e34b35c68a58
出典データセット
uspto-grants-2016_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US09394309B2

反応ノート

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