2-(Piperidin-4-yl)pyridine → (2R,3R)-2-(2,4-difluorophenyl)-3-(4-pyridin-2-ylpiperidin-1-yl)-1-(1,2,4-triazol-1-yl)butan-2-ol

HRID 1009062ノート

反応式

HRID 1009062 の反応式
[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C:9]1([CH2:13][N:14]2[CH:18]=[N:17][CH:16]=[N:15]2)[CH:11]([CH3:12])[O:10]1.[NH:19]1[CH2:24][CH2:23][CH:22]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=2)[CH2:21][CH2:20]1.O.O.O.Cl([O-])(=O)(=O)=O.[Li+]>C(#N)C>[F:1][C:2]1[CH:7]=[C:6]([F:8])[CH:5]=[CH:4][C:3]=1[C@:9]([OH:10])([C@H:11]([N:19]1[CH2:24][CH2:23][CH:22]([C:25]2[CH:30]=[CH:29][CH:28]=[CH:27][N:26]=2)[CH2:21][CH2:20]1)[CH3:12])[CH2:13][N:14]1[CH:18]=[N:17][CH:16]=[N:15]1

参加物

5

反応物 3

HCID 103747502-(Piperidin-4-yl)pyridineHCID 147064491-((2-(2,4-Difluorophenyl)-3-methyl-2-oxiranyl)methyl)-1H-1,2,4-triazoleHCID 23708903Lithium perchlorate trihydrate

生成物 1

HCID 44538601(2R,3R)-2-(2,4-difluorophenyl)-3-(4-pyridin-2-ylpiperidin-1-yl)-1-(1,2,4-triazol-1-yl)butan-2-ol収率 28.9%

試薬・触媒・溶媒 1

HCID 6342Acetonitrile溶媒

実験手順

(2R,3R)-2-(2,4-Difluorophenyl-3-methyl-2-(1H-1,2,4-triazol-1-ylmethyl)oxirane (0.76 g, 3.0 mmol) and 2-(4-piperidyl)pyridine (4.3 g, 26.5 mmol) were dissolved in acetonitrile (50 ml), and lithium perchlorate trihydrate (4.25 g, 26.5 mmol) was added thereto and refluxed for 40 hours. The solvent was evaporated under a reduced pressure, and the thus obtained residue was dissolved in ethyl acetate and washed with water. The solvent was again evaporated under a reduced pressure, and the residue was purified using a silica gel column to obtain 0.37 g of the intended substance (yield 28.9%).

後処理

  1. temperaturerefluxed for 40 hours
  2. customThe solvent was evaporated under a reduced pressure
  3. dissolutionthe thus obtained residue was dissolved in ethyl acetate
  4. washwashed with water
  5. customThe solvent was again evaporated under a reduced pressure
  6. customthe residue was purified
  7. customto obtain 0.37 g of the intended substance (yield 28.9%)

出典と根拠

ORDレコード
ord-d4250cb97f7d475aa01a91b29924fb11
出典データセット
uspto-grants-2011_07
特許番号
US07973056B2

反応ノート

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