Tetrahydrofuran → 7-bromo-4-methyl-1H-indole

HRID 1173087

反応式

HRID 1173087 の反応式
O1CCCC1.[CH:6]([Mg]Br)=[CH2:7].[Br:10][C:11]1[CH:16]=[CH:15][C:14]([CH3:17])=[CH:13][C:12]=1[N+:18]([O-])=O.[Cl-].[NH4+]>C(OCC)(=O)C>[Br:10][C:11]1[CH:16]=[CH:15][C:6]([CH3:7])=[C:13]2[C:12]=1[NH:18][CH:17]=[CH:14]2

参加物

6

反応物 4

HCID 8028Tetrahydrofuran2 回HCID 25517Ammonium ChlorideHCID 792244-Bromo-3-nitrotolueneHCID 178418507HCID 178418507、化合物

生成物 1

HCID 187528627-bromo-4-methyl-1H-indole

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

1 l (1 mol) of a tetrahydrofuran solution containing 1.0 M vinylmagnesium bromide was added to a tetrahydrofuran solution (300 ml) containing 65.0 g (301 mmol) of 2-bromo-5-methylnitrobenzene at −60° C. under stirring for one hour in nitrogen atmosphere. An aqueous saturated ammonium chloride and ethyl acetate were added to the reaction mixture solution, and the insoluble matters were filtered off. The filtrate was dried over magnesium sulfate and concentrated. Then, the residue was purified by silica gel column chromatography, to give 35.5 g of the title compound.

後処理

  1. filtrationthe insoluble matters were filtered off
  2. dry with materialThe filtrate was dried over magnesium sulfate
  3. concentrationconcentrated
  4. customThen, the residue was purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-dfbab5c697244738928f3dd8cc579791
出典データセット
uspto-grants-2010_11
特許番号
US07834049B2

関連ノート

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