Imidazole → HCID 66977751、化合物

HRID 1399943ノート

反応式

HRID 1399943 の反応式
[Br:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][CH:11]=1)[O:5][CH2:6][CH2:7][OH:8].N1C=CN=C1.[CH3:17][C:18]([Si:21](Cl)([CH3:23])[CH3:22])([CH3:20])[CH3:19]>ClCCl>[Br:1][C:2]1[CH:3]=[C:4]([CH:9]=[CH:10][CH:11]=1)[O:5][CH2:6][CH2:7][O:8][Si:21]([C:18]([CH3:20])([CH3:19])[CH3:17])([CH3:23])[CH3:22]

参加物

5

反応物 3

HCID 795ImidazoleHCID 28928tert-Butyldimethylsilyl chlorideHCID 105367272-(3-Bromophenoxy)ethanol

生成物 1

HCID 66977751HCID 66977751、化合物

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To a solution of 2-(3-Bromo-phenoxy)-ethanol (2.0 g, 9.2 mol) in dichloromethane (15 mL) at ice water bath temperature was added (1.25 g, 1.84 mmol) imidazole followed by the addition of TBSCl (1.67 g, 11 mmol) under nitrogen protection. TLC showed reaction was complete in 1 h. The reaction mixture was filtered. The filtrate was washed with water and dried over Na2SO4. The crude product was purified by column chromatography eluted with hexanes/ethyl acetate to afford titled product as a light color oil (2.65 g, 87%).

後処理

  1. customreaction
  2. filtrationThe reaction mixture was filtered
  3. washThe filtrate was washed with water
  4. dry with materialdried over Na2SO4
  5. customThe crude product was purified by column chromatography
  6. washeluted with hexanes/ethyl acetate

出典と根拠

ORDレコード
ord-2c71311c803c473a8c5b24b5c0f23521
出典データセット
uspto-grants-2014_12
特許番号
US08906909B2

反応ノート

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