Trifluoroacetic acid → HCID 18187489, 화합물

HRID 2303631노트

반응식

HRID 2303631 반응식
FC(F)(F)C(O)=O.C(OC([N:15]1[CH2:20][CH2:19][CH:18]([CH2:21][CH2:22][C:23]([F:31])([F:30])[C:24]2[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=2)[CH2:17][CH2:16]1)=O)(C)(C)C.C(=O)(O)[O-].[Na+].[OH-].[Na+]>C(Cl)Cl.O.[Cl-].[Na+].O.CCOCC>[F:31][C:23]([F:30])([C:24]1[CH:29]=[CH:28][CH:27]=[CH:26][CH:25]=1)[CH2:22][CH2:21][CH:18]1[CH2:17][CH2:16][NH:15][CH2:20][CH2:19]1

참가 물질

9

반응물 4

HCID 6422Trifluoroacetic acidHCID 14798Sodium HydroxideHCID 516892Sodium BicarbonateHCID 18187485HCID 18187485, 화합물

생성물 1

HCID 18187489HCID 18187489, 화합물

시약·촉매·용매 4

HCID 962Water용매HCID 3283Diethyl Ether용매HCID 6344Dichloromethane용매HCID 57417360Sodium chloride; water용매

실험 절차

Trifluoroacetic acid (2.5 mL, 3.7 g, 32 mmol) was added dropwise to a solution of 1-(t-butoxycarbonyl)-4-(3,3-difluoro-3-phenylprop-1-yl)piperidine from Step C (42 mg, 0.12 mmol) in methylene chloride (2.5 mL) at 0° C. After 80 min., the solution was transferred using a double-ended needle to a rapidly stirred solution of sodium bicarbonate (5.0 g, 60 mmol) in water (50 mL). Ether (50 mL) and 2.5 N aq. NaOH (20 mL) were added, followed by solid brine to saturate the aqueous layer. The aqueous layer was separated and extracted with ether (50 mL). The organic layers were washed in succession with saturated aq. brine (20 mL), combined, dried (sodium sulfate), decanted, and evaporated to give the title compound as 27 mg of colorless oil.

후처리

  1. concentrationto saturate the aqueous layer
  2. customThe aqueous layer was separated
  3. extractionextracted with ether (50 mL)
  4. washThe organic layers were washed in succession with saturated aq. brine (20 mL)
  5. dry with materialdried (sodium sulfate)
  6. customdecanted
  7. customevaporated

출처 및 근거

ORD 기록
ord-4112e08091a244a688a96b68f335ada2
출처 데이터셋
uspto-grants-2002_08
특허 번호
US06432981B1

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