Sodium Iodide → HCID 23370065、化合物

HRID 1901071ノート

反応式

HRID 1901071 の反応式
Br[CH2:2][CH2:3][CH2:4][C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:8]([OH:15])=[C:7]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:6]=1.[N+:20]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[OH:29])([O-:22])=[O:21].C(=O)([O-])[O-].[K+].[K+].[I-].[Na+]>CN(C)C=O.O>[N+:20]([C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][C:24]=1[O:29][CH2:2][CH2:3][CH2:4][C:5]1[CH:10]=[C:9]([C:11]([CH3:14])([CH3:13])[CH3:12])[C:8]([OH:15])=[C:7]([C:16]([CH3:19])([CH3:18])[CH3:17])[CH:6]=1)([O-:22])=[O:21]

参加物

7

反応物 4

HCID 5238Sodium IodideHCID 69472-NitrophenolHCID 11430Potassium CarbonateHCID 1900717Phenol, 4-(3-bromopropyl)-2,6-bis(1,1-dimethylethyl)-

生成物 1

HCID 23370065HCID 23370065、化合物収率 74.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6228Dimethylformamide溶媒

実験手順

A mixture of 4-(3-bromopropyl)-2,6-di-t-butylphenol (1.20 g), 2-nitrophenol (0.51 g), potassium carbonate (1.01 g) and a catalytic amount of sodium iodide was stirred in dimethylformamide (10 ml) at 60°-70° C. for 1.5 hrs. The reaction solution was poured into water, extracted with ethyl acetate, washed with water and then saturated saline, and dried over anhydrous MgSO4. After distilling off the solvent, the residue was purified by a silica gel column chromatography (hexane:ethyl acetate=10:1) to give 4-[3-(2-nitrophenoxy)propyl]-2,6-di-t-butylphenol (1.05 g, 74%).

後処理

  1. extractionextracted with ethyl acetate
  2. washwashed with water
  3. dry with materialsaturated saline, and dried over anhydrous MgSO4
  4. distillationAfter distilling off the solvent
  5. customthe residue was purified by a silica gel column chromatography (hexane:ethyl acetate=10:1)

出典と根拠

ORDレコード
ord-a1d008a519fd43189374a7c16e7ebb55
出典データセット
uspto-grants-1996_11
特許番号
US05576335

反応ノート

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