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HCID 474081, 화합물 → HCID 474087, 화합물

HRID 1857767
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HRID 1857767 반응식
C([O:4][CH2:5][CH2:6][N:7]1[C:11]([S:12][C:13]2[CH:18]=[C:17]([Cl:19])[CH:16]=[C:15]([Cl:20])[CH:14]=2)=[C:10]([CH:21]([CH3:23])[CH3:22])[N:9]=[C:8]1[CH2:24][CH2:25][O:26][CH2:27][C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1)(=O)C.[H-].[Al+3].[Li+].[H-].[H-].[H-]>C(OCC)C.O>[CH2:27]([O:26][CH2:25][CH2:24][C:8]1[N:7]([CH2:6][CH2:5][OH:4])[C:11]([S:12][C:13]2[CH:18]=[C:17]([Cl:19])[CH:16]=[C:15]([Cl:20])[CH:14]=2)=[C:10]([CH:21]([CH3:23])[CH3:22])[N:9]=1)[C:28]1[CH:33]=[CH:32][CH:31]=[CH:30][CH:29]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 474081HCID 474081, 화합물HCID 21226445Aluminium lithium hydride

생성물 1

HCID 474087HCID 474087, 화합물수율 91%

시약·촉매·용매 2

HCID 962Water용매HCID 3283Diethyl Ether용매

실험 절차

In 30 ml of dry diethyl ether was dissolved 3.0 g (5.9 mmol) of the ester compound (130c), followed by addition of 230 mg (6 mmol) of lithium aluminum hydride under ice-cooling, and the mixture was stirred at room temperature for 15 minutes. The mixture was diluted with water, extracted with ethyl acetate, the extract was washed with water, dried over anhydrous sodium sulfate, filtered, and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (ethyl acetate), and further recrystallized from ethyl acetate-n-hexane to give 2.5 g of 2-(2-(2-benzyloxyethyl)-5-(3,5-dichlorophenylthio)-4-isopropyl-1H-imidazol-1-yl)ethanol (130d) as crystals (yield 91%). mp 129-130° C.

후처리

  1. temperaturecooling
  2. extractionextracted with ethyl acetate
  3. washthe extract was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. filtrationfiltered
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was purified by silica gel column chromatography (ethyl acetate)
  8. customfurther recrystallized from ethyl acetate-n-hexane

출처 및 근거

ORD 기록
ord-24b3825846e145ec9e49e117df53d2b2
출처 데이터셋
uspto-grants-2000_11
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06147097

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