Sodium Hydroxide → HCID 22504616, 화합물

HRID 1368941노트

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HRID 1368941 반응식
[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

참가 물질

6

반응물 3

HCID 14798Sodium HydroxideHCID 73833Benzene, ((2-bromoethoxy)methyl)-HCID 22504600HCID 22504600, 화합물

생성물 1

HCID 22504616HCID 22504616, 화합물

시약·촉매·용매 2

HCID 74236Tetrabutylammonium Bromide촉매HCID 1140Toluene용매

반응 조건

온도
70 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-e5226fd6ae2349daa4042cb453151fb9
출처 데이터셋
uspto-grants-2003_06
특허 번호
US06576645B1

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