Ammonium Chloride → α,3-Dimethyl-4-pyridinemethanol

HRID 2092046ノート

反応式

HRID 2092046 の反応式
[CH3:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[CH:8]=[O:9].[CH3:10][Mg]Br.[Cl-].[NH4+]>O1CCCC1>[CH3:1][C:2]1[CH:3]=[N:4][CH:5]=[CH:6][C:7]=1[CH:8]([OH:9])[CH3:10]

参加物

5

反応物 3

HCID 25517Ammonium ChlorideHCID 15018803-Methyl-4-pyridinecarboxaldehydeHCID 178418573HCID 178418573、化合物

生成物 1

HCID 59574200α,3-Dimethyl-4-pyridinemethanol

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

3-Methylpyridine-4-carbaldehyde (310.6 mg, 1.00 mmol) in tetrahydrofuran (6 mL) was mixed with methylmagnesium bromide (0.98 M in tetrahydrofuran, 4.74 mL, 4.65 mmol) under −78° C., and the mixture was warmed slowly to room temperature for 16 hours with stirring. After completion of the reaction, the reaction solution was mixed with saturated aqueous ammonium chloride and extracted with ethyl acetate, and the organic layer was dried over anhydrous sodium sulfate and evaporated under reduced pressure. The resulting crude reaction product containing the desired product was used for the next step (310.6 mg).

後処理

  1. customAfter completion of the reaction
  2. extractionextracted with ethyl acetate
  3. dry with materialthe organic layer was dried over anhydrous sodium sulfate
  4. customevaporated under reduced pressure
  5. customThe resulting crude reaction product

出典と根拠

ORDレコード
ord-7bd446a8fcfb47f48736ffce306ac101
出典データセット
uspto-grants-2013_05
特許番号
US08440666B2

反応ノート

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