Water → 2-Nitro-5-(2-quinolylmethoxy)benzyl alcohol

HRID 1721684

反応式

HRID 1721684 の反応式
[OH:1][C:2]1[CH:3]=[CH:4][C:5]([N+:10]([O-:12])=[O:11])=[C:6]([CH:9]=1)[CH2:7][OH:8].O.[F-].C([N+](CC)(CC)CC)C.Cl[CH2:25][C:26]1[CH:35]=[CH:34][C:33]2[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=2)[N:27]=1.O>CN(C=O)C>[N+:10]([C:5]1[CH:4]=[CH:3][C:2]([O:1][CH2:25][C:26]2[CH:35]=[CH:34][C:33]3[C:28](=[CH:29][CH:30]=[CH:31][CH:32]=3)[N:27]=2)=[CH:9][C:6]=1[CH2:7][OH:8])([O-:12])=[O:11]

参加物

6

反応物 4

HCID 962WaterHCID 203942-(Chloromethyl)quinolineHCID 1089463-(Hydroxymethyl)-4-nitrophenolHCID 16211652Tetraethylammonium fluoride hydrate

生成物 1

HCID 106148772-Nitro-5-(2-quinolylmethoxy)benzyl alcohol収率 33.3%

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 5-hydroxy-2-nitrobenzyl alcohol (5.1 g, 30 mmol), tetraethylammonium fluoride hydrate (8.94 g, 60 mmol) and 2-chloromethylquinoline (5.31 g, 30 mmol) in DMF (90 ml) was stirred at room temperature for 72 hours. The reaction mixture was then poured into water and extracted with ethyl acetate. The extract was dried over MgSO4 and concentrated in vacuo. To the residue was added methylene chloride (25 ml) and the solid was filtered to provide 3.1 g of 2-nitro-5-(2-quinolylmethoxy)benzyl alcohol.

後処理

  1. extractionextracted with ethyl acetate
  2. dry with materialThe extract was dried over MgSO4
  3. concentrationconcentrated in vacuo
  4. additionTo the residue was added methylene chloride (25 ml)
  5. filtrationthe solid was filtered

出典と根拠

ORDレコード
ord-f345799dcf9c49f0851569fcf72688c4
出典データセット
uspto-grants-1996_04
特許番号
US05512581

関連ノート

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