Water → Benzene, 1-((2-(4-(difluoromethoxy)phenyl)-2-methylpropoxy)methyl)-3-phenoxy-

HRID 1589447노트

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HRID 1589447 반응식
[F:1][CH:2]([F:15])[O:3][C:4]1[CH:9]=[CH:8][C:7]([C:10]([CH3:14])([CH3:13])[CH2:11][OH:12])=[CH:6][CH:5]=1.[O:16]([C:23]1[CH:24]=[C:25]([CH:28]=[CH:29][CH:30]=1)[CH2:26]Cl)[C:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1.[OH-].[Na+].O>[Br-].C([N+](CC)(CC)CC1C=CC=CC=1)C.C1C=CC=CC=1>[F:1][CH:2]([F:15])[O:3][C:4]1[CH:5]=[CH:6][C:7]([C:10]([CH3:13])([CH3:14])[CH2:11][O:12][CH2:26][C:25]2[CH:28]=[CH:29][CH:30]=[C:23]([O:16][C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=3)[CH:24]=2)=[CH:8][CH:9]=1

참가 물질

7

반응물 4

HCID 962WaterHCID 14798Sodium HydroxideHCID 932913-Phenoxybenzyl chlorideHCID 15582647HCID 15582647, 화합물

생성물 1

HCID 3067125Benzene, 1-((2-(4-(difluoromethoxy)phenyl)-2-methylpropoxy)methyl)-3-phenoxy-수율 81%

시약·촉매·용매 2

HCID 165294Benzyltriethylammonium bromide촉매HCID 241Benzene용매

실험 절차

2.0 g of 2-(4-difluoromethoxyphenyl)-2-methylpropyl alcohol, 2.0 g of m-phenoxybenzyl chloride, 20 g of 50% NaOH and 0.3 g of triethylbenzyl ammonium bromide were stirred at 50° C. for 2 hours. Then, H2O and benzene were added to the reaction mixture, and the mixture was sufficiently shaken and the benzene layer was separated, washed with water, dried over Na2SO4, and evaporated under reduced pressure, and the obtained crude ether was purified by column chromatography on 130 g of silica gel (2:3 mixed solvent of toluene and hexane was used as eluent) to give 3.0 g of the desired ether (the yield was 81% of the theoretical yield).

후처리

  1. customthe benzene layer was separated
  2. washwashed with water
  3. dry with materialdried over Na2SO4
  4. customevaporated under reduced pressure
  5. customthe obtained crude ether
  6. customwas purified by column chromatography on 130 g of silica gel (2:3 mixed solvent of toluene and hexane was used as eluent)
  7. customto give 3.0 g of the desired ether (the yield was 81% of the
  8. customtheoretical yield)

출처 및 근거

ORD 기록
ord-e5c87c050b8144e09b8d5904b847eb0d
출처 데이터셋
uspto-grants-1986_02
특허 번호
US04570005

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