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1,2-Dichloroethane → 2-Methyl-N-(7-methyl-1H-indazol-5-yl)-6-oxo-4-[4-(trifluoromethyl)phenyl]-1,4,5,6-tetrahydro-3-pyridinecarboxamide

HRID 734683
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인쇄 미리보기

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HRID 734683 반응식
[F:1][C:2]([F:21])([F:20])[C:3]1[CH:8]=[CH:7][C:6]([CH:9]2[CH2:14][C:13](=[O:15])[NH:12][C:11]([CH3:16])=[C:10]2[C:17](O)=[O:18])=[CH:5][CH:4]=1.[NH2:22][C:23]1[CH:24]=[C:25]2[C:29](=[C:30]([CH3:32])[CH:31]=1)[NH:28][N:27]=[CH:26]2.C(Cl)CCl.CCN(CC)CC>CN(C=O)C.CCOC(C)=O.Cl>[CH3:16][C:11]1[NH:12][C:13](=[O:15])[CH2:14][CH:9]([C:6]2[CH:5]=[CH:4][C:3]([C:2]([F:20])([F:21])[F:1])=[CH:8][CH:7]=2)[C:10]=1[C:17]([NH:22][C:23]1[CH:24]=[C:25]2[C:29](=[C:30]([CH3:32])[CH:31]=1)[NH:28][N:27]=[CH:26]2)=[O:18]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 4

HCID 111,2-DichloroethaneHCID 8471TriethylamineHCID 13820227-methyl-1H-indazol-5-amineHCID 160998632-Methyl-6-oxo-4-(4-(trifluoromethyl)phenyl)-1,4,5,6-tetrahydropyridine-3-carboxylic acid

생성물 1

HCID 114645152-Methyl-N-(7-methyl-1H-indazol-5-yl)-6-oxo-4-[4-(trifluoromethyl)phenyl]-1,4,5,6-tetrahydro-3-pyridinecarboxamide수율 36%

시약·촉매·용매 3

HCID 313Hydrochloric Acid용매HCID 6228Dimethylformamide용매HCID 8857Ethyl Acetate용매

실험 절차

The product of Example 5, Step 2 (160 mg, 0.535 mmol, 1.00 equiv), 5-amino-7-methylindazole (79 mg, 0.535 mmol, 1.0 equiv), and EDC (123 mg, 0.642 mmol, 1.20 equiv) were suspended in 1.5 mL DMF. Et3N (0.089 mL, 0.642 mmol, 1.2 equiv) was added and the solution was stirred at room temperature for 18 hrs. The reaction mixture was diluted with EtOAc and 1N HCl. The phases were separated, and the organic phase was washed twice with 1N HCl, once with satd. NaHCO3, and once with satd. NaCl. The organic phase was dried over Na2SO4, filtered, and concentrated en vacuo. The residue was triturated with EtOAc and CH2Cl2, filtered, and washed with CH2Cl2 to provide 82 mg (36%) of the title compound as an off white solid. MS (ES+) m/e 429 [M+H]+

후처리

  1. customThe phases were separated
  2. washthe organic phase was washed twice with 1N HCl, once with satd
  3. dry with materialThe organic phase was dried over Na2SO4
  4. filtrationfiltered
  5. concentrationconcentrated en vacuo
  6. customThe residue was triturated with EtOAc and CH2Cl2
  7. filtrationfiltered
  8. washwashed with CH2Cl2

출처 및 근거

ORD 기록
ord-9257a2575b1540b38d53f70a99c88357
출처 데이터셋
uspto-grants-2009_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07592357B2

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