Trifluoroacetic acid → HCID 68734897、化合物

HRID 2382193ノート

反応式

HRID 2382193 の反応式
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

参加物

5

反応物 3

HCID 6422Trifluoroacetic acidHCID 8003PentaneHCID 68731553HCID 68731553、化合物

生成物 1

HCID 68734897HCID 68734897、化合物収率 69%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-0aa8e8178ad04e21bc50b43719d27ada
出典データセット
uspto-grants-2012_09
特許番号
US08258306B2

反応ノート

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