Hydrazine hydrate (1:1) → HCID 178461462, 화합물

HRID 657635노트

반응식

HRID 657635 반응식
[CH3:1][C@H:2]1[CH2:7][C@H:6]([CH3:8])[CH2:5][N:4]([CH2:9][CH2:10][CH2:11][O:12][C:13]2[CH:18]=[CH:17][C:16]([C:19](=O)[CH2:20][CH:21]=O)=[CH:15][CH:14]=2)[CH2:3]1.O.[NH2:25][NH2:26]>CO.O>[CH3:1][C@H:2]1[CH2:7][C@H:6]([CH3:8])[CH2:5][N:4]([CH2:9][CH2:10][CH2:11][O:12][C:13]2[CH:18]=[CH:17][C:16]([C:19]3[CH:20]=[CH:21][NH:26][N:25]=3)=[CH:15][CH:14]=2)[CH2:3]1

참가 물질

5

반응물 2

HCID 24654Hydrazine hydrate (1:1)HCID 86629974HCID 86629974, 화합물

생성물 1

HCID 178461462HCID 178461462, 화합물

시약·촉매·용매 2

HCID 887Methanol용매HCID 962Water용매

실험 절차

A solution of trans-3,5-dimethyl-1-{3-[4-(3-oxopropanoyl)phenoxy]propyl}-piperidine (200 mg) in a mixture of hydrazine hydrate (50 μL) and methanol (4 mL) is stirred for one hour at room temperature. The mixture is diluted with water and extracted twice with ethyl acetate, dried over magnesium sulphate, concentrated under reduced pressure and purified by chromatography over silica gel. Fractions containing the expected product are pooled, concentrated under reduced pressure and salted with oxalic acid to afford 142 mg of trans-3,5-dimethyl-1-{3-[4-(pyrazol-3-yl)phenoxy]propyl}piperidine, oxalate as a pale yellow solid.

후처리

  1. extractionextracted twice with ethyl acetate
  2. dry with materialdried over magnesium sulphate
  3. concentrationconcentrated under reduced pressure
  4. custompurified by chromatography over silica gel
  5. additionFractions containing the expected product
  6. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-c06562a4b9a64dfe816a532b26eaddf7
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08076329B2

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