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Hydrochloric Acid → 4-Hydroxy-1-methylpiperidine-4-carbonitrile

HRID 1734565
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반응식

HRID 1734565 반응식
[CH3:1][N:2]1[CH2:7][CH2:6][C:5](=[O:8])[CH2:4][CH2:3]1.Cl.[C-:10]#[N:11].[K+]>O>[OH:8][C:5]1([C:10]#[N:11])[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]1
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참가 물질

5

반응물 3

HCID 313Hydrochloric AcidHCID 9032Potassium CyanideHCID 740491-Methyl-4-piperidone

생성물 1

HCID 2840534-Hydroxy-1-methylpiperidine-4-carbonitrile수율 67%

시약·촉매·용매 1

HCID 962Water용매2회

반응 조건

온도
10 °C

실험 절차

To freshly distilled 1-methylpiperidin-4-one (81.72 g, 0.72 mole) in water (200 cc), were added about 100 cc HCl 37% to pH 3. The reaction mixture was cooled in an ice bath and potassium cyanide (49 g, 0.75 mole) in water (200 cc) was added at an adequate rate in order to maintain an internal temperature of about 10° C. The reaction was stirred two hours more after the addition and then filtered. After washing with water and drying, the product, 4-hydroxy-4-cyano-1-methylpiperidine, was obtained in 67% yield as a white powder (67 g, 0.48 mole, mp. 135° C.).

후처리

  1. temperatureThe reaction mixture was cooled in an ice bath
  2. additionmore after the addition
  3. filtrationfiltered
  4. washAfter washing with water
  5. customdrying

출처 및 근거

ORD 기록
ord-eb0b82aade02403387005403ea3040cf
출처 데이터셋
uspto-grants-1996_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05534520

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