Potassium Carbonate → 1-(2-Bromo-5-chlorobenzyloxy)-4-(2-methoxyethoxy)benzene

HRID 1360013ノート

反応式

HRID 1360013 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[CH2:9]Br.C([O-])([O-])=O.[K+].[K+].[CH3:17][O:18][CH2:19][CH2:20][O:21][C:22]1[CH:27]=[CH:26][C:25]([OH:28])=[CH:24][CH:23]=1>C(#N)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([Cl:8])=[CH:4][C:3]=1[CH2:9][O:28][C:25]1[CH:24]=[CH:23][C:22]([O:21][CH2:20][CH2:19][O:18][CH3:17])=[CH:27][CH:26]=1

参加物

5

反応物 3

HCID 11430Potassium CarbonateHCID 118465052-Bromo-5-chlorobenzyl bromideHCID 133135614-(2-Methoxyethoxy)phenol

生成物 1

HCID 669702041-(2-Bromo-5-chlorobenzyloxy)-4-(2-methoxyethoxy)benzene収率 95%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

1.42 g (5 mmol) of the compound obtained in Step 1 was dissolved in 20 ml of acetonitrile, 1.38 g (10 mmol) of K2CO3 and 0.84 g (5 mmol) of 4-(2-methoxyethoxy)phenol were added thereto, which was refluxed for 15 hours. The reaction mixture was distilled under a reduced pressure to remove the solvent, and 20 ml of ethyl acetate was added thereto. The resulting mixture was washed twice with water, dried over anhydrous MgSO4, and concentrated under a reduced pressure. The concentrate was subjected to column chromatography using 20% ethyl acetate/hexane to obtain 1.76 g (yield 95%) of 1-(2-bromo-5-chlorobenzyloxy)-4-(2-methoxyethoxy)benzene.

後処理

  1. temperaturewhich was refluxed for 15 hours
  2. distillationThe reaction mixture was distilled under a reduced pressure
  3. customto remove the solvent, and 20 ml of ethyl acetate
  4. additionwas added
  5. washThe resulting mixture was washed twice with water
  6. dry with materialdried over anhydrous MgSO4
  7. concentrationconcentrated under a reduced pressure

出典と根拠

ORDレコード
ord-4f723d9e911b4eb681e8df8a5aaebf65
出典データセット
uspto-grants-2011_02
特許番号
US07879835B2

反応ノート

読み込み中…