Water → HCID 58452692, 화합물

HRID 70687노트

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HRID 70687 반응식
Cl[Si](C)(C)C.[I-].[K+].[Cl:8][C:9]1[CH:10]=[CH:11][C:12](/[C:17](/[C:25]2[CH:30]=[CH:29][C:28]([CH2:31][OH:32])=[CH:27][CH:26]=2)=[CH:18]/[C@@H:19]2[NH:23][C:22](=[O:24])[CH2:21][CH2:20]2)=[N:13][C:14]=1[O:15]C.O>C(#N)C>[Cl:8][C:9]1[C:14](=[O:15])[NH:13][C:12](/[C:17](/[C:25]2[CH:26]=[CH:27][C:28]([CH2:31][OH:32])=[CH:29][CH:30]=2)=[CH:18]/[C@H:19]2[CH2:20][CH2:21][C:22](=[O:24])[NH:23]2)=[CH:11][CH:10]=1

참가 물질

6

반응물 4

HCID 962WaterHCID 4875Potassium IodideHCID 6397ChlorotrimethylsilaneHCID 67397484HCID 67397484, 화합물

생성물 1

HCID 58452692HCID 58452692, 화합물수율 14%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

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온도
60 °C

실험 절차

Chlorotrimethylsilane (0.123 mL) and potassium iodide (263 mg) were sequentially added to a solution of (5R)-5-{(E)-2-(5-chloro-6-methoxypyridin-2-yl)-2-[4-(hydroxymethyl)phenyl]ethenyl}pyrrolidin-2-one (142 mg) in acetonitrile (1.5 mL) at room temperature, after which the mixture was stirred at 60° C. for two hours. Water was added to the reaction solution, followed by extraction with ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate and filtered, after which the solvent was evaporated under reduced pressure. The residue was purified by silica gel chromatography (methanol:ethyl acetate=1:10) to give the title compound as a colorless solid (19 mg, 14%).

후처리

  1. extractionfollowed by extraction with ethyl acetate
  2. washThe organic layer was washed with water and brine
  3. dry with materialdried over anhydrous magnesium sulfate
  4. filtrationfiltered
  5. customafter which the solvent was evaporated under reduced pressure
  6. customThe residue was purified by silica gel chromatography (methanol:ethyl acetate=1:10)

출처 및 근거

ORD 기록
ord-2de7a1992787413c8f516be258f3f4d7
출처 데이터셋
uspto-grants-2014_09
특허 번호
US08822503B2

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