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Water → HCID 178520945, 화합물

HRID 1515110
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HRID 1515110 반응식
[F:1][C:2]([F:13])([F:12])[C@H:3]1[CH2:8][CH2:7][C@H:6]([C:9](O)=[O:10])[CH2:5][CH2:4]1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.[OH-].[Na+]>O1CCCC1>[F:1][C:2]([F:12])([F:13])[C@H:3]1[CH2:4][CH2:5][C@H:6]([CH2:9][OH:10])[CH2:7][CH2:8]1
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6

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HCID 962Water2회HCID 14798Sodium HydroxideHCID 21226445Aluminium lithium hydrideHCID 178525710HCID 178525710, 화합물

생성물 1

HCID 178520945HCID 178520945, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

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온도
0 °C

실험 절차

trans-4-(Trifluoromethyl)cyclohexanecarboxylic acid (1.5 g, 7.65 mmol) was dissolved in tetrahydrofuran (20 mL). The reaction solution was cooled to 0° C., and lithium aluminum hydride (435 mg, 11.5 mmol) was added thereto, and then, the resulting mixture was stirred at room temperature for 3 hours. The reaction solution was cooled to 0° C., and water (0.4 mL), a 5 N aqueous solution of sodium hydroxide (0.4 mL), and water (1.2 mL) were added thereto, followed by filtration. To the filtrate, ethyl acetate was added, and the organic layer was washed with a saturated aqueous solution of sodium hydrogen carbonate and a saturated sodium chloride solution, then dried over anhydrous magnesium sulfate and filtered. Then, the solvent was distilled off under reduced pressure, whereby a crude product was obtained as a colorless oily substance (1.18 g).

후처리

  1. temperatureThe reaction solution was cooled to 0° C.
  2. filtrationfollowed by filtration
  3. additionTo the filtrate, ethyl acetate was added
  4. washthe organic layer was washed with a saturated aqueous solution of sodium hydrogen carbonate
  5. dry with materiala saturated sodium chloride solution, then dried over anhydrous magnesium sulfate
  6. filtrationfiltered
  7. distillationThen, the solvent was distilled off under reduced pressure, whereby a crude product
  8. customwas obtained as a colorless oily substance (1.18 g)

출처 및 근거

ORD 기록
ord-1b28a4facd854401b2c9a5ea8edbb5e4
출처 데이터셋
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08222281B2

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