Sodium Hydroxide → HCID 22504616、化合物

HRID 1368941ノート

反応式

HRID 1368941 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][C:9]([C:11]2[CH:16]=[CH:15][C:14]([O:17][CH2:18][CH2:19][N:20]([CH3:22])[CH3:21])=[CH:13][CH:12]=2)=[O:10])=[CH:4][CH:3]=1.[OH-].[Na+].Br[CH2:26][CH2:27][O:28][CH2:29][C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1>CCCC[N+](CCCC)(CCCC)CCCC.[Br-].C1(C)C=CC=CC=1>[CH2:29]([O:28][CH2:27][CH2:26][CH:8]([C:5]1[CH:6]=[CH:7][C:2]([Cl:1])=[CH:3][CH:4]=1)[C:9]([C:11]1[CH:16]=[CH:15][C:14]([O:17][CH2:18][CH2:19][N:20]([CH3:21])[CH3:22])=[CH:13][CH:12]=1)=[O:10])[C:30]1[CH:35]=[CH:34][CH:33]=[CH:32][CH:31]=1

参加物

6

反応物 3

HCID 14798Sodium HydroxideHCID 73833Benzene, ((2-bromoethoxy)methyl)-HCID 22504600HCID 22504600、化合物

生成物 1

HCID 22504616HCID 22504616、化合物

試薬・触媒・溶媒 2

HCID 74236Tetrabutylammonium Bromide触媒HCID 1140Toluene溶媒

反応条件

温度
70 °C

実験手順

The mixture containing 2-(4-chlorophenyl)-1-[4-(2-dimethylaminoethoxy)phenyl]ethanone (6.3 g, 0.020 mol) and TBABr (0.5 g) in toluene (70 ml) is heated to 70° C. and 48% aqueous sodium hydroxide (70 ml) is added. The mixture is stirred for 30 min. and (2-bromoethoxymethyl)benzene (5.5 g, 0.025 mol) is added dropwise at 85-90° C. The reaction mixture is stirred at 95-100° C. for 3 h. The layers are separated and the aqueous phase is extracted with toluene. The combined organic phases are washed with water and the solvent is evaporated. The residual product (9.0 g) is used in the next reaction step without further purification.

後処理

  1. stirringThe reaction mixture is stirred at 95-100° C. for 3 h
  2. customThe layers are separated
  3. extractionthe aqueous phase is extracted with toluene
  4. washThe combined organic phases are washed with water
  5. customthe solvent is evaporated
  6. customThe residual product (9.0 g) is used in the next reaction step without further purification

出典と根拠

ORDレコード
ord-e5226fd6ae2349daa4042cb453151fb9
出典データセット
uspto-grants-2003_06
特許番号
US06576645B1

反応ノート

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