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Benzyl Bromide → HCID 15000227、化合物

HRID 396122
ノート
印刷プレビュー

反応式

HRID 396122 の反応式
C(=O)([O-])[O-].[K+].[K+].[OH:7][C:8]1[CH:15]=[CH:14][C:11]([CH:12]=[O:13])=[C:10]([N+:16]([O-:18])=[O:17])[CH:9]=1.[CH2:19](Br)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1>CN(C=O)C>[CH2:19]([O:7][C:8]1[CH:15]=[CH:14][C:11]([CH:12]=[O:13])=[C:10]([N+:16]([O-:18])=[O:17])[CH:9]=1)[C:20]1[CH:25]=[CH:24][CH:23]=[CH:22][CH:21]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 7498Benzyl BromideHCID 11430Potassium CarbonateHCID 5861374-Hydroxy-2-nitrobenzaldehyde

生成物 1

HCID 15000227HCID 15000227、化合物収率 99.4%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

8.51 g (61.57 mmol) of potassium carbonate are added to a solution of 10.0 g (58.64 mmol) of 4-hydroxy-2-nitrobenzaldehyde in 70 ml of DMF. The solution is briefly stirred, then 10.53 g (61.57 mmol) of benzyl bromide are added and the reaction mixture is stirred at room temperature for 3 h. The resulting solid is then filtered off, 250 ml of water are added to the filtrate and the aqueous phase is extracted 3× with ethyl acetate. The organic phase is washed twice with water, dried over sodium sulphate, concentrated in vacuo and the residue is dried. 15.0 g (99%) of 4-benzyloxy-2-nitrobenzaldehyde are obtained as a yellow solid.

後処理

  1. stirringthe reaction mixture is stirred at room temperature for 3 h
  2. filtrationThe resulting solid is then filtered off
  3. addition250 ml of water are added to the filtrate
  4. extractionthe aqueous phase is extracted 3× with ethyl acetate
  5. washThe organic phase is washed twice with water
  6. dry with materialdried over sodium sulphate
  7. concentrationconcentrated in vacuo
  8. customthe residue is dried

出典と根拠

ORDレコード
ord-f540cf9a013244a58f7effce7f6193f4
出典データセット
uspto-grants-2003_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06608049B2

反応ノート

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