tert-Butyl acetate → Di-tert-butyl ether

HRID 388630

反応式

HRID 388630 の反応式
IC1C=[CH:10][C:9]2[C:4](=CC=C[CH:8]=2)N=1.C([O:15][C:16]([CH3:19])([CH3:18])[CH3:17])(=O)C>C(Cl)Cl.CCOC(C)=O>[C:16]([O:15][C:9]([CH3:8])([CH3:4])[CH3:10])([CH3:19])([CH3:18])[CH3:17]

参加物

5

反応物 2

HCID 10908tert-Butyl acetateHCID 810442-Iodoquinoline

生成物 1

HCID 22541Di-tert-butyl ether収率 71%

試薬・触媒・溶媒 2

HCID 6344Dichloromethane溶媒HCID 8857Ethyl Acetate溶媒

実験手順

HClO4 (1.17 mL, 13.6 mmol) is added to a suspension of 48k (3.40 g, 9.06 mmol) in t-butyl acetate (100 mL) and DCM (150 mL). The reaction mixture is stirred at RT overnight then is diluted with EtOAc (150 mL). The solution is washed twice with aqueous 5% NaHCO3 solution, dried (MgSO4), filtered and concentrated under reduced pressure. The residue is purified by flash chromatography (Combi-Flash; EtOAc/hexane) to give t-butylether 481 (2.76 g, 71% yield) as a white solid.

後処理

  1. washThe solution is washed twice with aqueous 5% NaHCO3 solution
  2. dry with materialdried (MgSO4)
  3. filtrationfiltered
  4. concentrationconcentrated under reduced pressure
  5. customThe residue is purified by flash chromatography (Combi-Flash; EtOAc/hexane)

出典と根拠

ORDレコード
ord-1caa156855f54569842fc1528fd2f9ae
出典データセット
uspto-grants-2013_02
特許番号
US08377960B2

関連ノート

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