Trifluoromethanesulfonic acid → HCID 13920595、化合物

HRID 569205ノート

反応式

HRID 569205 の反応式
[CH3:1][N:2]1[CH2:7][CH2:6][CH:5]([C:8]([CH:10]2[CH:15]([CH2:16][CH2:17][C:18]3[CH:23]=[CH:22][CH:21]=[C:20]([F:24])[CH:19]=3)[CH2:14][CH2:13][CH2:12][NH:11]2)=O)[CH2:4][CH2:3]1.FC(F)(F)S(O)(=O)=O>>[F:24][C:20]1[CH:21]=[CH:22][C:23]2[C:8](=[C:5]3[CH2:6][CH2:7][N:2]([CH3:1])[CH2:3][CH2:4]3)[C:10]3=[N:11][CH:12]=[CH:13][CH:14]=[C:15]3[CH2:16][CH2:17][C:18]=2[CH:19]=1

参加物

3

反応物 2

HCID 62406Trifluoromethanesulfonic acidHCID 20148818HCID 20148818、化合物

生成物 1

HCID 13920595HCID 13920595、化合物収率 38%

実験手順

A solution of (1-methyl-4-piperidinyl)[3-[2-(3-fluorophenyl)ethyl]-2-piperidinyl]methanone (15.0 g, 0.046 mole) in 74 mL (125.5 g, 0.837 mole) of trifluoromethanesulfonic acid is stirred at ambient temperature for 18 hours. The reaction is quenched with ice-water and the solution made basic with potassium hydroxide. The product is extracted into ethyl acetate. The ethyl acetate solution is filtered to remove insolubles and the filtrate is concentrated to a residue. Following purification by silica gel chromatography, 5.4 g (0.0175 mole) of product is obtained in 38% yield.

後処理

  1. customThe reaction is quenched with ice-water
  2. extractionThe product is extracted into ethyl acetate
  3. filtrationThe ethyl acetate solution is filtered
  4. customto remove insolubles
  5. concentrationthe filtrate is concentrated to a residue
  6. custompurification by silica gel chromatography

出典と根拠

ORDレコード
ord-189722dad6644dd8a6ab93610b5cf63d
出典データセット
uspto-grants-1988_03
特許番号
US04731447

反応ノート

読み込み中…