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Pyridine → N-Isoxazol-3-yl-4-methyl-3-[7-(2-morpholin-4-ylethoxy)-1-oxoisoquinolin-2(1H)-yl]benzamide

HRID 506985
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HRID 506985 반응식
[CH3:1][C:2]1[CH:10]=[CH:9][C:5]([C:6]([OH:8])=O)=[CH:4][C:3]=1[N:11]1[CH:20]=[CH:19][C:18]2[C:13](=[CH:14][C:15]([O:21][CH2:22][CH2:23][N:24]3[CH2:29][CH2:28][O:27][CH2:26][CH2:25]3)=[CH:16][CH:17]=2)[C:12]1=[O:30].C(Cl)(=O)C(Cl)=O.N1C=CC=CC=1.[NH2:43][C:44]1[CH:48]=[CH:47][O:46][N:45]=1>C(Cl)Cl.CN(C=O)C.C(OCC)(=O)C>[O:46]1[CH:47]=[CH:48][C:44]([NH:43][C:6](=[O:8])[C:5]2[CH:9]=[CH:10][C:2]([CH3:1])=[C:3]([N:11]3[CH:20]=[CH:19][C:18]4[C:13](=[CH:14][C:15]([O:21][CH2:22][CH2:23][N:24]5[CH2:29][CH2:28][O:27][CH2:26][CH2:25]5)=[CH:16][CH:17]=4)[C:12]3=[O:30])[CH:4]=2)=[N:45]1
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참가 물질

8

반응물 4

HCID 1049PyridineHCID 65578Oxalyl chlorideHCID 18102163-IsoxazolamineHCID 670185774-Methyl-3-[7-(2-morpholin-4-ylethoxy)-1-oxoisoquinolin-2(1H)-yl]benzoic acid

생성물 1

HCID 11496557N-Isoxazol-3-yl-4-methyl-3-[7-(2-morpholin-4-ylethoxy)-1-oxoisoquinolin-2(1H)-yl]benzamide

시약·촉매·용매 3

HCID 6228
Dimethylformamide
촉매
HCID 6344Dichloromethane용매
HCID 8857Ethyl Acetate용매

실험 절차

4-Methyl-3-[7-(2-morpholin-4-ylethoxy)-1-oxoisoquinolin-2(1H)-yl]benzoic acid (708 mg) was dissolved in methylene chloride (5 ml) and DMF (3 drops) and cooled to 0° C. under an argon atmosphere. Oxalyl chloride (0.33 ml) was added and the reaction mixture stirred at room temperature for 2 hours. Pyridine (1.45 ml) and 3-aminoisoxazole (0.64 ml) were added and the reaction mixture stirred at room temperature for 2 hours. The reaction mixture was diluted with ethyl acetate, washed with 1N NaOH, dried (magnesium sulfate) and concentrated. Purification by column chromatography on an ion exchange column (isolute SCX column from International Sorbent Technology Limited, Henoed, Mid-Glamorgan, UK) using initially methanol and then a 99:1 mixture of methanol and aqueous ammonia solution to give an oily solid. The solid was triturated with ethyl acetate to give N-Isoxazol-3-yl-4-methyl-3-[7-(2-morpholin-4-ylethoxy)-1-oxoisoquinolin-2(1H)-yl]benzamide as a white solid (70 mg); NMR Spectrum: (DMSOd6) 2.15 (s, 3H), 2.50 (m, 4H), 2.75 (m, 2H), 3.55 (m, 4H), 4.20 (m, 2H), 6.75 (m, 1H), 7.05 (m, 1H), 7.25 (m, 1H), 7.45 (m, 1H), 7.60 (m, 1H), 7.70 (m, 2H), 8.00 (m, 2H), 8.85 (s, 1H), 11.45 (s, 1H); Mass Spectrum: M+H+ 475.

후처리

  1. stirringthe reaction mixture stirred at room temperature for 2 hours
  2. washwashed with 1N NaOH
  3. dry with materialdried (magnesium sulfate)
  4. concentrationconcentrated
  5. customPurification by column chromatography on an ion exchange column (isolute SCX column from International Sorbent Technology Limited, Henoed, Mid-Glamorgan, UK)
  6. additiona 99:1 mixture of methanol and aqueous ammonia solution
  7. customto give an oily solid
  8. customThe solid was triturated with ethyl acetate

출처 및 근거

ORD 기록
ord-7480050905bb427e9ee8a1a9ff748635
출처 데이터셋
uspto-grants-2010_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07786115B2

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