Chloromethyl Methyl Ether → 2-Benzyl-1-methoxymethyloxy-4-iodobenzene

HRID 2216349

反応式

HRID 2216349 の反応式
[CH2:1]([C:8]1[CH:13]=[C:12]([I:14])[CH:11]=[CH:10][C:9]=1[OH:15])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.[CH3:16][O:17][CH2:18]Cl.O1CCCC1.[H-].[Na+]>O>[CH2:1]([C:8]1[CH:13]=[C:12]([I:14])[CH:11]=[CH:10][C:9]=1[O:15][CH2:16][O:17][CH3:18])[C:2]1[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=1

参加物

6

反応物 4

HCID 7864Chloromethyl Methyl EtherHCID 8028TetrahydrofuranHCID 24758Sodium hydrideHCID 219422992-Benzyl-4-iodophenol

生成物 1

HCID 219423042-Benzyl-1-methoxymethyloxy-4-iodobenzene

試薬・触媒・溶媒 1

HCID 962Water溶媒

実験手順

10.1 g of 2-benzyl-1-hydroxy-4-iodobenzene and 3 ml of chloromethyl methyl ether were added to 100 ml of tetrahydrofuran and while stirring on an ice bath, 1.45 g of 60% (oily) sodium hydride was added dropwise to the mixture. After stirring for 2 hours, water was added to the reaction mixture, which then was extracted with ethyl acetate, washed with saturated brine and thereafter dried over anhydrous magnesium sulfate. The solvent was removed, and the residue was purified by silica gel column chromatography with 10% ethyl acetate/hexane, to give 8.7 g of the title compound.

後処理

  1. stirringAfter stirring for 2 hours
  2. extractionthen was extracted with ethyl acetate
  3. washwashed with saturated brine
  4. dry with materialdried over anhydrous magnesium sulfate
  5. customThe solvent was removed
  6. customthe residue was purified by silica gel column chromatography with 10% ethyl acetate/hexane

出典と根拠

ORDレコード
ord-d1ca98b4f2744c7490f5e8fb06c967dd
出典データセット
uspto-grants-2006_09
特許番号
US07112593B2

関連ノート

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