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1-Methylpiperazine → HCID 67382819, 화합물

HRID 1896289
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HRID 1896289 반응식
Cl[C:2]1[CH:7]=[C:6]([CH2:8][C:9]([O:11]C(C)(C)C)=O)[CH:5]=[CH:4][N:3]=1.[CH3:16][N:17]1[CH2:22][CH2:21][NH:20][CH2:19][CH2:18]1>O>[CH3:16][N:17]1[CH2:22][CH2:21][N:20]([C:9](=[O:11])[CH2:8][C:6]2[CH:5]=[CH:4][N:3]=[C:2]([N:20]3[CH2:21][CH2:22][N:17]([CH3:16])[CH2:18][CH2:19]3)[CH:7]=2)[CH2:19][CH2:18]1
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참가 물질

4

반응물 2

HCID 531671-MethylpiperazineHCID 86623474HCID 86623474, 화합물

생성물 1

HCID 67382819HCID 67382819, 화합물수율 71%

시약·촉매·용매 1

HCID 962Water용매

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온도
140 °C

실험 절차

A suspension of tert-butyl 2-(2-chloropyridin-4-yl)acetate (600 mg, 2.64 mmol) and N-methyl piperazine (2 ml) was heated in a sealed tube for 24 h at 140° C. The reaction mixture was cooled to room temperature, water was added and extracted with DCM. The combined organic layer was washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated under vacuum to get the crude product. Purification by column chromatography over neutral alumina using 5% MeOH in CHCl3 as eluent afforded 600 mg (71%) of 1-(4-methylpiperazin-1-yl)-2-(2-(4-methylpiperazin-1-yl)pyridin-4-yl)ethanone as colorless liquid.

후처리

  1. temperatureThe reaction mixture was cooled to room temperature
  2. extractionextracted with DCM
  3. washThe combined organic layer was washed with brine
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under vacuum
  7. customto get the crude product
  8. customPurification by column chromatography over neutral alumina using 5% MeOH in CHCl3 as eluent

출처 및 근거

ORD 기록
ord-a981b80d0e4d495cadddf64565921c5c
출처 데이터셋
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08518948B2

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