Triethylamine → 4-(4-Nitrophenoxy)phenyl 2-(4-(4-chlorophenoxy)phenoxy)propionate

HRID 1110664ノート

反応式

HRID 1110664 の反応式
[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:18]=[CH:17][C:10]([O:11][CH:12]([CH3:16])[C:13](Cl)=[O:14])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1.[N+:21]([C:24]1[CH:37]=[CH:36][C:27]([O:28][C:29]2[CH:34]=[CH:33][C:32]([OH:35])=[CH:31][CH:30]=2)=[CH:26][CH:25]=1)([O-:23])=[O:22].C(N(CC)CC)C>O1CCCC1>[Cl:1][C:2]1[CH:20]=[CH:19][C:5]([O:6][C:7]2[CH:18]=[CH:17][C:10]([O:11][CH:12]([CH3:16])[C:13]([O:35][C:32]3[CH:31]=[CH:30][C:29]([O:28][C:27]4[CH:36]=[CH:37][C:24]([N+:21]([O-:23])=[O:22])=[CH:25][CH:26]=4)=[CH:34][CH:33]=3)=[O:14])=[CH:9][CH:8]=2)=[CH:4][CH:3]=1

参加物

5

反応物 3

HCID 8471TriethylamineHCID 1524504-(4-Nitrophenoxy)phenolHCID 129528252-(4-(4-Chlorophenoxy)phenoxy)propionic acid chloride

生成物 1

HCID 144985654-(4-Nitrophenoxy)phenyl 2-(4-(4-chlorophenoxy)phenoxy)propionate収率 82%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

2-(4-(4-Chlorophenoxy)phenoxy)propionic acid chloride (0.6 g) and 4-(4-nitrophenoxy)phenol (0.5 g) were dissolved in dry tetrahydrofuran (10 ml), and the solution was stirred with an addition of triethylamine (0.3 ml) at room temperature for 2 hours. After completion of the reaction, the solvent was evaporated under a reduced pressure, the residue was dissolved in methylene chloride (20 ml), and washed with 1N hydrochloric acid, water, saturated aqueous sodium hydrogen carbonate, water, and aqueous saturated sodium chloride. After drying over anhydrous magnesium sulfate, the solvent was evaporated and the residue obtained was purified by medium pressure column chromatography to obtain 4-(4-nitrophenoxy)phenyl 2-(4-(4-chlorophenoxy)phenoxy)propionate (0.8 g)

後処理

  1. customAfter completion of the reaction
  2. customthe solvent was evaporated under a reduced pressure
  3. dissolutionthe residue was dissolved in methylene chloride (20 ml)
  4. washwashed with 1N hydrochloric acid, water, saturated aqueous sodium hydrogen carbonate, water, and aqueous saturated sodium chloride
  5. dry with materialAfter drying over anhydrous magnesium sulfate
  6. customthe solvent was evaporated
  7. customthe residue obtained
  8. customwas purified by medium pressure column chromatography

出典と根拠

ORDレコード
ord-2e3a2c44b1124f1a983ae1dd4804c019
出典データセット
uspto-grants-1990_12
特許番号
US04976773

反応ノート

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