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

HRID 984158
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HRID 984158 반응식
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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
90 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d0e91faf873849f6a5fa6ddb05acdae5
출처 데이터셋
uspto-grants-2005_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06867221B2

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