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

HRID 1452120

反応式

HRID 1452120 の反応式
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

参加物

7

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

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 further 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 further stirred vigorously for 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.

後処理

  1. stirringThe two-phase mixture is further stirred vigorously for 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)

出典と根拠

ORDレコード
ord-33cd66e359274b39bed0b012229ef622
出典データセット
uspto-grants-1997_02
特許番号
US05606078

関連ノート

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