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Benzenesulfonyl chloride → [4-amino-7-bromo-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-imidazo[4,5-c]quinolin-2-yl]methanol

HRID 81915
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HRID 81915 반응식
C([O:4][CH2:5][C:6]1[N:7]([CH2:20][CH:21]2[CH2:26][CH2:25][O:24][CH2:23][CH2:22]2)[C:8]2[C:17]3[CH:16]=[CH:15][C:14]([Br:18])=[CH:13][C:12]=3[N:11]=[CH:10][C:9]=2[N:19]=1)(=O)C.C(=O)(O)[O-].[Na+].[OH-].[NH4+:33].C1(S(Cl)(=O)=O)C=CC=CC=1>O.C(Cl)(Cl)Cl>[NH2:33][C:10]1[C:9]2[N:19]=[C:6]([CH2:5][OH:4])[N:7]([CH2:20][CH:21]3[CH2:26][CH2:25][O:24][CH2:23][CH2:22]3)[C:8]=2[C:17]2[CH:16]=[CH:15][C:14]([Br:18])=[CH:13][C:12]=2[N:11]=1
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참가 물질

7

반응물 4

HCID 7369Benzenesulfonyl chloride2회HCID 14923Ammonium Hydroxide2회HCID 516892Sodium Bicarbonate2회HCID 67281006[7-bromo-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-imidazo[4,5-c]quinolin-2-yl]methyl acetate

생성물 1

HCID 67281118[4-amino-7-bromo-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-imidazo[4,5-c]quinolin-2-yl]methanol수율 52.1%

시약·촉매·용매 2

HCID 962Water용매HCID 6212Chloroform용매

실험 절차

3-Chloroperoxybenozic acid (2.4 g, 50% pure, 7.0 mmol) was added to a mixture of [7-bromo-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-imidazo[4,5-c]quinolin-2-yl]methyl acetate (2.3 g, 5.4 mmol) and chloroform (27 mL) at ambient temperature. The reaction was stirred at this temperature for 18 hours. Saturated aqueous sodium bicarbonate (50 mL) and water (50 mL) were then added to the reaction and the layers were separated. The aqueous layer was extracted with additional dichloromethane. The organic layers were combined, dried over sodium sulfate, and concentrated under reduced pressure to a dark oil. This oil was dissolved in methanol (27 mL) and to this solution was added 15 M ammonium hydroxide (3.6 mL, 54 mmol) and benzene sulfonyl chloride (2.9 mL, 23 mmol). The resulting reaction mixture was stirred at ambient temperature for 2 hours before adding additional 15 M ammonium hydroxide (3.6 mL, 54 mmol) and benzene sulfonyl chloride (2.9 mL, 23 mmol). The reaction was stirred 18 hours. The reaction was then concentrated under reduced pressure and diluted with saturated aqueous sodium bicarbonate and chloroform. A suspension resulted that was filtered to afford a solid that was stirred with saturated aqueous sodium bicarbonate and filtered to give 1.1 g of [4-amino-7-bromo-1-(tetrahydro-2H-pyran-4-ylmethyl)-1H-imidazo[4,5-c]quinolin-2-yl]methanol as a white solid.

후처리

  1. customthe layers were separated
  2. extractionThe aqueous layer was extracted with additional dichloromethane
  3. dry with materialdried over sodium sulfate
  4. concentrationconcentrated under reduced pressure to a dark oil
  5. dissolutionThis oil was dissolved in methanol (27 mL) and to this solution
  6. customThe resulting reaction mixture
  7. stirringwas stirred at ambient temperature for 2 hours
  8. stirringThe reaction was stirred 18 hours
  9. concentrationThe reaction was then concentrated under reduced pressure
  10. additiondiluted with saturated aqueous sodium bicarbonate and chloroform
  11. customA suspension resulted
  12. filtrationthat was filtered
  13. customto afford a solid
  14. filtrationfiltered

출처 및 근거

ORD 기록
ord-29d3b249ab3f4cb4852dacdc42184268
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08846710B2

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