(Diethylamino)sulfur trifluoride → 2-Bromo-4-(1-fluorocyclopropyl)-1-methoxybenzene

HRID 406397ノート

反応式

HRID 406397 の反応式
C(N(S(F)(F)[F:7])CC)C.[Br:10][C:11]1[CH:12]=[C:13]([C:19]2(O[Si](C)(C)C)[CH2:21][CH2:20]2)[CH:14]=[CH:15][C:16]=1[O:17][CH3:18]>ClCCl.O>[Br:10][C:11]1[CH:12]=[C:13]([C:19]2([F:7])[CH2:21][CH2:20]2)[CH:14]=[CH:15][C:16]=1[O:17][CH3:18]

参加物

5

反応物 2

HCID 123472(Diethylamino)sulfur trifluorideHCID 66618984[1-(3-Bromo-4-methoxyphenyl)cyclopropyloxy]trimethylsilane

生成物 1

HCID 666334672-Bromo-4-(1-fluorocyclopropyl)-1-methoxybenzene

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 6344Dichloromethane溶媒

実験手順

Diethylaminosulfur trifluoride (2.4 ml) was added to a solution of [1-(3-bromo-4-methoxyphenyl)cyclopropyloxy]trimethylsilane (3.84 g) in dichloromethane (68 ml). The reaction mixture was stirred at room temperature for 2.5 hours. The reaction mixture was diluted with water and extracted with ethyl acetate. The organic layer was washed with brine and dried over anhydrous magnesium sulfate. The filtrate was concentrated under reduced pressure and the residue was purified by silica gel column chromatography to obtain the title compound (1.88 g).

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. concentrationThe filtrate was concentrated under reduced pressure
  5. customthe residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-726dfb4c1ab8487dba67ae08046d3264
出典データセット
uspto-grants-2014_06
特許番号
US08754100B2

反応ノート

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