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Ammonium Chloride → 1-(4-Ethoxy-2,3-difluorophenyl)-4-(3-propylcyclopentyl)cyclohexanol

HRID 2358887
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HRID 2358887 반응식
Br[C:2]1[CH:7]=[CH:6][C:5]([O:8][CH2:9][CH3:10])=[C:4]([F:11])[C:3]=1[F:12].C([Li])CCC.[CH2:18]([CH:21]1[CH2:25][CH2:24][CH:23]([CH:26]2[CH2:31][CH2:30][C:29](=[O:32])[CH2:28][CH2:27]2)[CH2:22]1)[CH2:19][CH3:20].[Cl-].[NH4+]>C1COCC1.CCCCCC>[CH2:9]([O:8][C:5]1[CH:6]=[CH:7][C:2]([C:29]2([OH:32])[CH2:28][CH2:27][CH:26]([CH:23]3[CH2:24][CH2:25][CH:21]([CH2:18][CH2:19][CH3:20])[CH2:22]3)[CH2:31][CH2:30]2)=[C:3]([F:12])[C:4]=1[F:11])[CH3:10]
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참가 물질

7

반응물 4

HCID 25517Ammonium ChlorideHCID 269854911-Bromo-4-ethoxy-2,3-difluorobenzeneHCID 679922824-(3-Propylcyclopentyl)-cyclohexanoneHCID 178418339Butyllithium

생성물 1

HCID 679923521-(4-Ethoxy-2,3-difluorophenyl)-4-(3-propylcyclopentyl)cyclohexanol수율 94.7%

시약·촉매·용매 2

HCID 8028
Tetrahydrofuran
용매
2회
HCID 8058Hexane용매

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온도
-78 °C

실험 절차

THF (100 ml) was added to 1-bromo-4-ethoxy-2,3-difluorobenzene(5.1 g) in a reaction vessel under an atmosphere of nitrogen, and the mixture was cooled to −78° C. n-Butyllithium (1.57 M, in a hexane solution) (13.8 ml) was added dropwise at a temperature of −70° C. or lower. The stirring was continued at −78° C. for another 2 hours, and 4-(3-propylcyclopentyl)-cyclohexanone (3.0 g) in a THF (10 ml) solution was added dropwise at a temperature of −70° C. or lower. After the mixture had been stirred at −78° C. for another 1 hour, it was warmed to room temperature, and a saturated aqueous solution of ammonium chloride (50 ml) was added. The mixture was separated, and the water layer was extracted with ethyl acetate three times, and then the combined organic layer was washed with brine. The solution was dried over anhydrous magnesium sulfate and the solvent was distilled off under reduced pressure. The residue was purified by silica gel chromatography (eluent: ethyl acetate/n-heptane= 1/9 by volume) to give 1-(4-ethoxy-2,3-difluorophenyl)-4-(3-propylcyclopentyl)cyclohexanol (5.0 g).

후처리

  1. temperatureit was warmed to room temperature
  2. customThe mixture was separated
  3. extractionthe water layer was extracted with ethyl acetate three times
  4. washthe combined organic layer was washed with brine
  5. dry with materialThe solution was dried over anhydrous magnesium sulfate
  6. distillationthe solvent was distilled off under reduced pressure
  7. customThe residue was purified by silica gel chromatography (eluent: ethyl acetate/n-heptane= 1/9 by volume)

출처 및 근거

ORD 기록
ord-68b31ef77df246b59bf6f6bed1b04037
출처 데이터셋
uspto-grants-2014_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08685274B2

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