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Hydrochloric Acid → HCID 178491793, 화합물

HRID 77562
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HRID 77562 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][N:5]1[C:10]([C:11]2[CH:16]=[C:15]([F:17])[CH:14]=[CH:13][C:12]=2[O:18][CH3:19])=[CH:9][C:8](=[O:20])[NH:7][C:6]1=[S:21].[N:22]1([C:31]([N:33]2[CH2:36][C:35]([F:38])([F:37])[CH2:34]2)=N)C2C=CC=CC=2N=N1.C(N(CC)C(C)C)(C)C.Cl>CN(C=O)C.O1CCOCC1>[F:37][C:35]1([F:38])[CH2:36][N:33]([C:31](=[NH:22])[NH:1][CH2:2][CH2:3][CH2:4][N:5]2[C:10]([C:11]3[CH:16]=[C:15]([F:17])[CH:14]=[CH:13][C:12]=3[O:18][CH3:19])=[CH:9][C:8](=[O:20])[NH:7][C:6]2=[S:21])[CH2:34]1
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참가 물질

7

반응물 4

HCID 313Hydrochloric AcidHCID 81531DiisopropylethylamineHCID 866847021-(1H-Benzotriazol-1-yl)-1-(3,3-difluoroazetidin-1-yl)methanimineHCID 866847051-(3-aminopropyl)-6-(5-fluoro-2-methoxyphenyl)-2-thioxo-2,3-dihydropyrimidin-4(1H)-one

생성물 1

HCID 178491793HCID 178491793, 화합물수율 33%

시약·촉매·용매 2

HCID 6228
Dimethylformamide
용매
HCID 312751,4-Dioxane용매

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온도
60 °C

실험 절차

To a mixture of 1-(3-aminopropyl)-6-(5-fluoro-2-methoxyphenyl)-2-thioxo-2,3-dihydropyrimidin-4(1H)-one (prepared in an analogous manner to Example 6; 50 mg, 0.14 mmol) and 1-(1H-benzotriazol-1-yl)-1-(3,3-difluoroazetidin-1-yl)methanimine (47.5 mg, 0.174 mmol) in DMF (0.46 mL) was added N,N-diisopropylethylamine (0.061 mL, 0.35 mmol) under nitrogen and heated at 60° C. under nitrogen for 1 h. The reaction mixture was cooled to room temperature, and treated with 4N HCl in dioxane (0.25 mL). The mixture was stirred at room temperature for 10 min, then concentrated in vacuo and azeotroped with heptanes (3×10 mL). The residue was dissolved in water (1 mL) and purified using medium pressure reverse-phase (C18) chromatography (100:0 to 70:30 water/acetonitrile) to give the title compound as a white solid (22 mg, 33%).

후처리

  1. customprepared in an analogous manner to Example 6
  2. temperatureThe reaction mixture was cooled to room temperature
  3. concentrationconcentrated in vacuo
  4. customazeotroped with heptanes (3×10 mL)
  5. dissolutionThe residue was dissolved in water (1 mL)
  6. custompurified

출처 및 근거

ORD 기록
ord-74ea1dc27ef04c4b9640ba733c30884e
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08841314B2

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