Imidazole → ((4-Bromo-2-fluorobenzyl)oxy)(tert-butyl)dimethylsilane

HRID 564066ノート

反応式

HRID 564066 の反応式
[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][OH:9])=[C:4]([F:10])[CH:3]=1.[C:11]([Si:15](Cl)([CH3:17])[CH3:16])([CH3:14])([CH3:13])[CH3:12].N1C=CN=C1>CN(C=O)C.CN(C1C=CN=CC=1)C>[Br:1][C:2]1[CH:7]=[CH:6][C:5]([CH2:8][O:9][Si:15]([C:11]([CH3:14])([CH3:13])[CH3:12])([CH3:17])[CH3:16])=[C:4]([F:10])[CH:3]=1

参加物

6

反応物 3

HCID 795ImidazoleHCID 28928tert-Butyldimethylsilyl chlorideHCID 2734027(4-Bromo-2-fluorophenyl)methanol

生成物 1

HCID 57685175((4-Bromo-2-fluorobenzyl)oxy)(tert-butyl)dimethylsilane

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6228Dimethylformamide溶媒

実験手順

To 5.10 g (24.9 mmol) (4-bromo-2-fluoro-phenyl)-methanol in 30 mL DMF is added subsequently 4.06 g (26.1 mmol) tert-butyl-chloro-dimethyl silane, 2.57 g (37.3 mmol) imidazole and 456 mg (3.73 mmol) DMAP. The reaction mixture is stirred overnight at RT and the solvent is evaporated. The residue is diluted with EtOAc, washed five times with water and the combined organic phase is dried over MgSO4, filtered and the solvent is evaporated.

後処理

  1. customthe solvent is evaporated
  2. additionThe residue is diluted with EtOAc
  3. washwashed five times with water
  4. dry with materialthe combined organic phase is dried over MgSO4
  5. filtrationfiltered
  6. customthe solvent is evaporated

出典と根拠

ORDレコード
ord-a98381fd4d3e47f8843aab2a67915d97
出典データセット
uspto-grants-2011_11
特許番号
US08067590B2

反応ノート

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