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Triethylamine → HCID 66866322, 화합물

HRID 2194412
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HRID 2194412 반응식
Cl[C:2]1[C:3](=[O:15])[N:4]([CH3:14])[N:5]=[CH:6][C:7]=1[N:8]1[CH:12]=[CH:11][N:10]=[C:9]1[CH3:13].C(N(CC)CC)C>C(O)C.[Pd]>[CH3:14][N:4]1[C:3](=[O:15])[CH:2]=[C:7]([N:8]2[CH:12]=[CH:11][N:10]=[C:9]2[CH3:13])[CH:6]=[N:5]1
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참가 물질

5

반응물 2

HCID 8471TriethylamineHCID 668649334-chloro-2-methyl-5-(2-methyl-imidazol-1-yl)-2H-pyridazin-3-one

생성물 1

HCID 66866322HCID 66866322, 화합물수율 82.2%

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 702Ethanol용매

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온도
50 °C

실험 절차

To a solution of 3.30 g (14.7 mmol) of 4-chloro-2-methyl-5-(2-methyl-imidazol-1-yl)-2H-pyridazin-3-one in 60 ml of ethanol at 50° C. were added 2.44 ml (1.78 g, 17.6 mmol) of triethylamine and 0.312 g of Pd 10%/C. The suspension was stirred under hydrogen atmosphere for 15 h at 50° C. The catalyst was filtered off and washed twice with 10 ml of ethanol. The filtrate was concentrated in vaccuo, and taken up in 50 ml of methylene chloride. The organic phase was washed four times with water, dried and concentrated to yield the title compound (2.30 g, 12.09 mmol, 82%) as a white crystalline solid, MS: m/e=191.2 (M+H+).

후처리

  1. filtrationThe catalyst was filtered off
  2. washwashed twice with 10 ml of ethanol
  3. concentrationThe filtrate was concentrated in vaccuo
  4. washThe organic phase was washed four times with water
  5. customdried
  6. concentrationconcentrated

출처 및 근거

ORD 기록
ord-8dbf26cd37f442459f189d21d49ad45f
출처 데이터셋
uspto-grants-2012_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08334287B2

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