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Water → HCID 58452882, 화합물

HRID 70592
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인쇄 미리보기

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HRID 70592 반응식
C(=O)([O-])[O-].[K+].[K+].[CH2:7]([NH:9][CH2:10][CH3:11])[CH3:8].CC1C=CC(S(O[CH2:23][CH2:24][CH2:25][S:26][C:27]2[CH:32]=[CH:31][C:30](/[C:33](/[C:40]3[NH:41][C:42](=[O:47])[C:43]([CH3:46])=[CH:44][CH:45]=3)=[CH:34]\[CH:35]3[CH2:39][CH2:38][CH2:37][CH2:36]3)=[CH:29][C:28]=2[Cl:48])(=O)=O)=CC=1.O>C(#N)C>[Cl:48][C:28]1[CH:29]=[C:30](/[C:33](/[C:40]2[NH:41][C:42](=[O:47])[C:43]([CH3:46])=[CH:44][CH:45]=2)=[CH:34]\[CH:35]2[CH2:39][CH2:38][CH2:37][CH2:36]2)[CH:31]=[CH:32][C:27]=1[S:26][CH2:25][CH2:24][CH2:23][N:9]([CH2:10][CH3:11])[CH2:7][CH3:8]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

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6

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HCID 962WaterHCID 8021DiethylamineHCID 11430Potassium CarbonateHCID 866580093-({2-chloro-4-[(E)-2-cyclopentyl-1-(5-methyl-6-oxo-1,6-dihydropyridin-2-yl)ethenyl]phenyl}sulfanyl)propyl 4-methylbenzenesulfonate

생성물 1

HCID 58452882HCID 58452882, 화합물수율 66%

시약·촉매·용매 1

HCID 6342
Acetonitrile
용매

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온도
90 °C

실험 절차

Potassium carbonate (290 mg) and diethylamine (219 μL) were sequentially added to a solution of 3-({2-chloro-4-[(E)-2-cyclopentyl-1-(5-methyl-6-oxo-1,6-dihydropyridin-2-yl)ethenyl]phenyl}sulfanyl)propyl 4-methylbenzenesulfonate (33 mg) in acetonitrile (3 mL), and the mixture was stirred at 90° C. for two hours. The reaction solution was poured into water, followed by extraction with chloroform. The organic layer was washed with brine, dried over anhydrous magnesium sulfate and filtered. The solvent was then evaporated under reduced pressure. The residue was purified by silica gel column chromatography (chloroform:methanol=10:0→9:1) to give the title compound (18 mg, 66%) as a colorless amorphous.

후처리

  1. extractionfollowed by extraction with chloroform
  2. washThe organic layer was washed with brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customThe solvent was then evaporated under reduced pressure
  6. customThe residue was purified by silica gel column chromatography (chloroform:methanol=10:0→9:1)

출처 및 근거

ORD 기록
ord-0872360e61274ce2ae560dd1bd10dfcd
출처 데이터셋
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08822503B2

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