Hydrochloric Acid → HCID 66743562, 화합물

HRID 1620813

반응식

HRID 1620813 반응식
[F-].C([N+](CCCC)(CCCC)CCCC)CCC.[N:19]1[CH:24]=[CH:23][C:22]([C:25]2[CH:32]=[CH:31][CH:30]=[CH:29][C:26]=2[CH:27]=[O:28])=[CH:21][CH:20]=1.[F:33][C:34]([Si](C)(C)C)([F:36])[F:35].Cl>C1COCC1>[F:33][C:34]([F:36])([F:35])[CH:27]([C:26]1[CH:29]=[CH:30][CH:31]=[CH:32][C:25]=1[C:22]1[CH:23]=[CH:24][N:19]=[CH:20][CH:21]=1)[OH:28]

참가 물질

6

반응물 4

HCID 313Hydrochloric AcidHCID 552549(Trifluoromethyl)trimethylsilaneHCID 6428502-(4-Pyridinyl)benzaldehydeHCID 2724141Tetrabutylammonium Fluoride

생성물 1

HCID 66743562HCID 66743562, 화합물수율 43.4%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

Tetrabutylammonium fluoride (0.027 ml; 1.0 M solution in tetrahydrofuran) was added to a solution of 2-pyridin-4-yl-benzaldehyde (500 mg, 2.73 mmol) and trifluoromethyltrimethylsilane (TMSCF3) (485 μl, 3.28 mmol) in 5 ml of THF at 0° C. The formed mixture was warmed up to room temperature and stirred at room temperature for 4 hours. The reaction mixture was then treated with 5 ml of 1N HCl and stirred at room temperature overnight. The solvent was evaporated to dryness, 9 ml of 1M sodium carbonate aqueous solution was added, the aqueous phase was extracted with chloroform (3×10 ml), and the combined organic layer was washed with water, dried over MgSO4. The organic solvent was evaporated to give 300 mg of 2,2,2-trifluoro-1-(2-pyridin-4-yl-phenyl)ethanol, yield: 43%.

후처리

  1. stirringstirred at room temperature overnight
  2. customThe solvent was evaporated to dryness, 9 ml of 1M sodium carbonate aqueous solution
  3. additionwas added
  4. extractionthe aqueous phase was extracted with chloroform (3×10 ml)
  5. washthe combined organic layer was washed with water
  6. dry with materialdried over MgSO4
  7. customThe organic solvent was evaporated

출처 및 근거

ORD 기록
ord-ee69783d0a7c467087e93e0aa4975a7f
출처 데이터셋
uspto-grants-2014_07
특허 번호
US08772482B2

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