Chloromethyl Methyl Ether → 4-Bromo-2-(2-methoxymethoxyethyl)-anisole

HRID 1779807

반응식

HRID 1779807 반응식
C(N(C(C)C)C(C)C)C.[CH3:10][O:11][CH2:12]Cl.[Br:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[C:17]([CH2:23][CH2:24][OH:25])[CH:16]=1.[OH-].[NH4+]>ClCCl.O>[Br:14][C:15]1[CH:20]=[CH:19][C:18]([O:21][CH3:22])=[C:17]([CH2:23][CH2:24][O:25][CH2:10][O:11][CH3:12])[CH:16]=1

참가 물질

7

반응물 4

HCID 7864Chloromethyl Methyl EtherHCID 14923Ammonium HydroxideHCID 81531DiisopropylethylamineHCID 15020172-(5-Bromo-2-methoxyphenyl)ethan-1-ol

생성물 1

HCID 214585954-Bromo-2-(2-methoxymethoxyethyl)-anisole

시약·촉매·용매 2

HCID 962Water용매HCID 6344Dichloromethane용매

실험 절차

1.48 g of N-ethyl-diisopropylamine and 0.49 g of chlorodimethyl ether are added at room temperature to a solution of 948 mg of 4-bromo-2-(2-hydroxyethyl)-anisole in 30 ml of dichloromethane. The reaction mixture is stirred for 200 minutes at room temperature, and then 1 ml of water and 1 ml of 25% ammonium hydroxide solution are added thereto. The two-phase mixture is stirred vigorously for a further 15 minutes and then the organic phase is separated off, dried over sodium sulfate and concentrated by evaporation. Purification of the residue by means of FC (hexane/dichloromethane=1:1) yields the title compound: Rf (dichloromethane)=0.6; HPLC Rt =17.33 minutes.

후처리

  1. stirringThe two-phase mixture is stirred vigorously for a further 15 minutes
  2. customthe organic phase is separated off
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated by evaporation
  5. customPurification of the residue by means of FC (hexane/dichloromethane=1:1)

출처 및 근거

ORD 기록
ord-196e086d435340a394c81c57ea6c1d0c
출처 데이터셋
uspto-grants-1997_05
특허 번호
US05627182

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