Ammonium Chloride → 1-(3-Bromophenyl)-2,2-dimethylpropan-1-ol

HRID 546831ノート

反応式

HRID 546831 の反応式
[C:1]([Mg]Cl)([CH3:4])([CH3:3])[CH3:2].[Br:7][C:8]1[CH:9]=[C:10]([CH:13]=[CH:14][CH:15]=1)[CH:11]=[O:12].[Cl-].[NH4+]>O1CCCC1>[Br:7][C:8]1[CH:9]=[C:10]([CH:11]([OH:12])[C:1]([CH3:4])([CH3:3])[CH3:2])[CH:13]=[CH:14][CH:15]=1

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 765833-BromobenzaldehydeHCID 178418310HCID 178418310、化合物

生成物 1

HCID 574434831-(3-Bromophenyl)-2,2-dimethylpropan-1-ol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

t-Butylmagnesium chloride (0.93 mol/l solution in tetrahydrofuran, 75.5 mL, 70.26 mmol) was added to a solution of 3-bromobenzaldehyde (10 g, 54.05 mmol) in tetrahydrofuran (100 mL) in a nitrogen atmosphere at −78° C. The mixture was stirred at the same temperature for one hour and then heated to room temperature. The reaction mixture was poured into a saturated aqueous ammonium chloride solution, followed by extraction with ethyl acetate. The extract was washed with brine and dried over anhydrous magnesium sulfate and filtered, and the solvent was distilled off under reduced pressure to give crude 1-(3-bromo-phenyl)-2,2-dimethyl-propan-1-ol.

後処理

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe extract was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. distillationthe solvent was distilled off under reduced pressure

出典と根拠

ORDレコード
ord-25a0da022fc04485a7bd82c0bcbed3fc
出典データセット
uspto-grants-2011_05
特許番号
US07935688B2

反応ノート

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