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Water → 2-Chloro-thieno[3,2-d]pyrimidine-7-carboxylic acid(2,4-dimethoxy-phenyl)-amide

HRID 1773620
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HRID 1773620 반응식
[Cl:1][C:2]1[N:3]=[CH:4][C:5]2[S:10][CH:9]=[C:8]([C:11]([OH:13])=O)[C:6]=2[N:7]=1.[CH:14](N(CC)C(C)C)(C)C.CN(C)[CH:25]=[O:26].C1CN(C(ON2N=[N:47][C:46]3[C:41]2=[CH:42][CH:43]=[CH:44][CH:45]=3)=[N+]2CCCC2)CC1.F[P-](F)(F)(F)(F)F.[OH2:56]>ClCCl>[CH3:14][O:56][C:41]1[CH:42]=[C:43]([O:26][CH3:25])[CH:44]=[CH:45][C:46]=1[NH:47][C:11]([C:8]1[C:6]2[N:7]=[C:2]([Cl:1])[N:3]=[CH:4][C:5]=2[S:10][CH:9]=1)=[O:13]
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참가 물질

7

반응물 5

HCID 962WaterHCID 6228DimethylformamideHCID 81531DiisopropylethylamineHCID 13685355O-(Benzotriazol-1-yl)-N,N,N',N'-bis(tetramethylene)uronium HexafluorophosphateHCID 580563052-Chlorothieno[3,2-D]pyrimidine-7-carboxylic acid

생성물 1

HCID 870961102-Chloro-thieno[3,2-d]pyrimidine-7-carboxylic acid(2,4-dimethoxy-phenyl)-amide

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 0.050 g (0.233 mmole) 2-chloro-thieno[3,2-d]pyrimidine-7-carboxylic acid, 0.0714 g (0.466 mmole) of 1-methyl-1H-benzol[d]imidazol-4-amine, 0.122 mL (0.699 mmole) of N,N-diisopropylethylamine and 1.55 mL of dimethylformamide was added 0.111 g (0.256 mmole) of O-(benzotriazol-1-yl)-N,N,N′,N′-bis(tetramethylene)uronium hexafluorophosphate. The mixture was stirred at room temperature for over night. Water and dichloromethane were added. The aqueous layer was washed three times with dichloromethane. The combined organic layer was washed with aqueous sodium carbonate, brine, dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure. Purification by silica gel chromatography, eluting with hexanes-ethyl acetate (gradient 100:0-60:40) gave 0.050 g of 2-chloro-thieno[3,2-d]pyrimidine-7-carboxylic acid(2,4-dimethoxy-phenyl)-amide as a yellow solid.

후처리

  1. washThe aqueous layer was washed three times with dichloromethane
  2. washThe combined organic layer was washed with aqueous sodium carbonate, brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated under reduced pressure
  6. customPurification by silica gel chromatography
  7. washeluting with hexanes-ethyl acetate (gradient 100:0-60:40)

출처 및 근거

ORD 기록
ord-de8a801c0548420089accb5b23f64418
출처 데이터셋
uspto-grants-2016_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US09255110B2

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