Trifluoroacetic acid → HCID 68734897, 화합물

HRID 2382193노트

반응식

HRID 2382193 반응식
O[C:2]([C:26]1[CH:31]=[CH:30][CH:29]=[CH:28][CH:27]=1)([C:16]1[CH:21]=[CH:20][C:19]([C:22]([F:25])([F:24])[F:23])=[CH:18][CH:17]=1)[CH:3]1[CH2:8][CH2:7][N:6](C(OC(C)(C)C)=O)[CH2:5][CH2:4]1.C(O)(C(F)(F)F)=O.CCCCC>C(Cl)Cl>[C:26]1([C:2]([C:16]2[CH:17]=[CH:18][C:19]([C:22]([F:25])([F:23])[F:24])=[CH:20][CH:21]=2)=[C:3]2[CH2:4][CH2:5][NH:6][CH2:7][CH2:8]2)[CH:27]=[CH:28][CH:29]=[CH:30][CH:31]=1

참가 물질

5

반응물 3

HCID 6422Trifluoroacetic acidHCID 8003PentaneHCID 68731553HCID 68731553, 화합물

생성물 1

HCID 68734897HCID 68734897, 화합물수율 69%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of tert-butyl 4-(hydroxy(phenyl)(4-(trifluoromethyl)phenyl)methyl)piperidine-1-carboxylate (1.0 g, 2.29 mmol) in dry DCM (10 mL) at 0° C. was added TFA (10 mL) dropwise and the resulting solution was stirred at rt for 16 h. The solvents were removed under vacuum. The residue was diluted with DCM, washed with sodium bicarbonate solution and water, dried over sodium sulfate and concentrated under vacuum to afford crude compound which was crashed out of pentane to give 4-(phenyl(4-(trifluoromethyl)phenyl)-methylene)piperidine (0.5 g, 69%) as a grey solid. MS (ESI, pos. ion) m/z: 318 (M+1).

후처리

  1. customThe solvents were removed under vacuum
  2. additionThe residue was diluted with DCM
  3. washwashed with sodium bicarbonate solution and water
  4. dry with materialdried over sodium sulfate
  5. concentrationconcentrated under vacuum
  6. customto afford crude compound which

출처 및 근거

ORD 기록
ord-0aa8e8178ad04e21bc50b43719d27ada
출처 데이터셋
uspto-grants-2012_09
특허 번호
US08258306B2

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