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Piperazine → N,2,6-Trimethyl-4-piperazin-1-yl-pyridine-3-carboxamide

HRID 333965
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HRID 333965 반응식
Cl[C:2]1[CH:7]=[C:6]([CH3:8])[N:5]=[C:4]([CH3:9])[C:3]=1[C:10]([NH:12][CH3:13])=[O:11].[NH:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1>N1C=CC=CC=1>[CH3:13][NH:12][C:10]([C:3]1[C:4]([CH3:9])=[N:5][C:6]([CH3:8])=[CH:7][C:2]=1[N:14]1[CH2:19][CH2:18][NH:17][CH2:16][CH2:15]1)=[O:11]
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참가 물질

4

반응물 2

HCID 4837PiperazineHCID 668359274-Chloro-N,2,6-trimethyl-pyridine-3-carboxamide

생성물 1

HCID 66835676N,2,6-Trimethyl-4-piperazin-1-yl-pyridine-3-carboxamide수율 75%

시약·촉매·용매 1

HCID 1049Pyridine용매

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온도
180 °C

실험 절차

4-Chloro-N,2,6-trimethyl-pyridine-3-carboxamide (300 mg, 1.5 mmol) was mixed with piperazine (645 mg, 7.5 mmol) and pyridine (3 ml) and heated under microwave irridation at 180° C. for 15 minutes. The solvent was removed under reduced pressure, the residue was taken up in 0.5 M NaOH saturated with sodium chloride and extracted with dichloromethane (2×). The combined extracts were dried over sodium sulfate, the solvent was evaporated under reduced pressure to yield 280 mg of a yellow solid (1.1 mmol, 75%). NMR (1H, 300 MHz, CD3CN): 6.73 (s, 1H), 6.70 (s, 1H), 2.99-3.02 (m, 4H), 2.82-2.86 (m, 7H), 2.37 (s, 3H), 2.35 (s, 3H).

후처리

  1. customThe solvent was removed under reduced pressure
  2. extractionextracted with dichloromethane (2×)
  3. dry with materialThe combined extracts were dried over sodium sulfate
  4. customthe solvent was evaporated under reduced pressure

출처 및 근거

ORD 기록
ord-8fa8229a15ee41458b82f5b0ec57cb41
출처 데이터셋
uspto-grants-2014_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08883791B2

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