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Water → 4-(4-Methyl-1-piperidinyl)benzoic acid

HRID 1354775
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HRID 1354775 반응식
[CH3:1][CH:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:15]=[CH:14][C:11]([C:12]#N)=[CH:10][CH:9]=2)[CH2:4][CH2:3]1.[OH-:16].[K+].[OH2:18]>C(O)CO>[CH3:1][CH:2]1[CH2:7][CH2:6][N:5]([C:8]2[CH:15]=[CH:14][C:11]([C:12]([OH:18])=[O:16])=[CH:10][CH:9]=2)[CH2:4][CH2:3]1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 3

HCID 962Water2회HCID 14797Potassium HydroxideHCID 31520804-(4-Methyl-piperidin-1-yl)-benzonitrile

생성물 1

HCID 6548094-(4-Methyl-1-piperidinyl)benzoic acid

시약·촉매·용매 1

HCID 174Ethylene Glycol용매

실험 절차

4-(4-Methylpiperidin1-yl)benzonitrile (1.2 g) was heated to reflux with potassium hydroxide (0.7 g) in water (2 ml) and ethylene glycol (8 ml) for 3 hours. The mixture was diluted with water, washed with ethyl acetate and acidified with 2N hydrochloric acid. The precipitated product was filtered off with suction, dissolved in dichloromethane, dried over sodium sulfate, concentrated and crystallized from diethyl ether. This resulted in the product with the molecular weight of 219.29 (C13H17NO2); MS(ESI): 220 (M+H+).

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후처리

  1. washwashed with ethyl acetate
  2. filtrationThe precipitated product was filtered off with suction
  3. dissolutiondissolved in dichloromethane
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated
  6. customcrystallized from diethyl ether
  7. customThis resulted in the product with the molecular weight of 219.29 (C13H17NO2)

출처 및 근거

ORD 기록
ord-09bf709467f24213b3fa62997fb2af80
출처 데이터셋
uspto-grants-2007_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07223788B2

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