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Hydrochloric Acid → [2-(3,4,5-Trimethoxyphenyl)pyridin-4-yl]methyl-4-piperidone

HRID 984158
ノート
印刷プレビュー

反応式

HRID 984158 の反応式
C1O[C:4]2([CH2:9][CH2:8][N:7]([CH2:10][C:11]3[CH:16]=[CH:15][N:14]=[C:13]([C:17]4[CH:22]=[C:21]([O:23][CH3:24])[C:20]([O:25][CH3:26])=[C:19]([O:27][CH3:28])[CH:18]=4)[CH:12]=3)[CH2:6][CH2:5]2)[O:3]C1.Cl.[OH-].[Na+]>C1COCC1>[CH3:24][O:23][C:21]1[CH:22]=[C:17]([C:13]2[CH:12]=[C:11]([CH2:10][N:7]3[CH2:6][CH2:5][C:4](=[O:3])[CH2:9][CH2:8]3)[CH:16]=[CH:15][N:14]=2)[CH:18]=[C:19]([O:27][CH3:28])[C:20]=1[O:25][CH3:26]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 213388351-[[2-(3,4,5-Trimethoxyphenyl)pyridin-4-yl]methyl]-4-piperidone ethylene ketal

生成物 1

HCID 22557811[2-(3,4,5-Trimethoxyphenyl)pyridin-4-yl]methyl-4-piperidone

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

反応条件

温度
90 °C

実験手順

To a solution of 1-[[2-(3,4,5-trimethoxyphenyl)pyridin-4-yl]methyl]-4-piperidone ethylene ketal (19.0 g) in THF (200 mL) was added 1 M hydrochloric acid (200 mL). The mixture was stirred at 90° C. overnight, then neutralized with 2 M sodium hydroxide and extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate and evaporated. The residual oil was applied to a column of silica gel using chloroform-methanol (40:1) as an eluent. Fractions containing the product were collected and evaporated to give the title compound.

後処理

  1. extractionextracted with ethyl acetate
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customevaporated
  5. additionFractions containing the product
  6. customwere collected
  7. customevaporated

出典と根拠

ORDレコード
ord-d0e91faf873849f6a5fa6ddb05acdae5
出典データセット
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06867221B2

反応ノート

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