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Triethylamine → [4,5-Dimethyl-6-((R)-3-methyl-piperazin-1-yl)-pyridazin-3-yl]-pyridin-3-yl-methanone

HRID 447087
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HRID 447087 반응식
Cl[C:2]1[N:7]=[N:6][C:5]([C:8]([C:10]2[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=2)=[O:9])=[C:4]([CH3:16])[C:3]=1[CH3:17].[CH3:18][C@@H:19]1[CH2:24][NH:23][CH2:22][CH2:21][NH:20]1.C(N(CC)CC)C>CN1C(=O)CCC1>[CH3:16][C:4]1[C:3]([CH3:17])=[C:2]([N:23]2[CH2:22][CH2:21][NH:20][C@H:19]([CH3:18])[CH2:24]2)[N:7]=[N:6][C:5]=1[C:8]([C:10]1[CH:11]=[N:12][CH:13]=[CH:14][CH:15]=1)=[O:9]
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참가 물질

5

반응물 3

HCID 8471TriethylamineHCID 73304342-Methylpiperazine, (R)-HCID 59191601HCID 59191601, 화합물

생성물 1

HCID 59191636[4,5-Dimethyl-6-((R)-3-methyl-piperazin-1-yl)-pyridazin-3-yl]-pyridin-3-yl-methanone수율 90%

시약·촉매·용매 1

HCID 13387N-methyl-2-pyrrolidone용매

실험 절차

(6-Chloro-4,5-dimethyl-pyridazin-3-yl)-pyridin-3-yl-methanone (1.2 g, 4.84 mmol) and (R)-2-methyl-piperazine (485 mg, 4.84 mmol) are added to a microwave vial followed by NMP (17 mL) and triethylamine (2.01 mL, 14.49 mmol). The vial is sealed and irradiated in the microwave at 170° C. for 30 min. The crude material is directly purified via flash chromatography on silica gel (0-20% methanol in CH2Cl2). The resulting oil is co-evaporated with CH2Cl2 and heptane to afford the title compound as a powder (1350 mg, 90%).

후처리

  1. customThe vial is sealed
  2. customirradiated in the microwave at 170° C. for 30 min
  3. customThe crude material is directly purified via flash chromatography on silica gel (0-20% methanol in CH2Cl2)

출처 및 근거

ORD 기록
ord-249db867cad0430a81ae8e7f68add546
출처 데이터셋
uspto-grants-2013_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08481542B2

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