Trifluoromethanesulfonic acid → HCID 13920595、化合物

HRID 2351566ノート

反応式

HRID 2351566 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-(3fluorophenyl)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 o (0.0175 mole) of oroduct 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, 5.4 o (0.0175 mole) of oroduct
  7. customis obtained in 38% yield

出典と根拠

ORDレコード
ord-bebb494a9a254e25a648f785be3e36b9
出典データセット
uspto-grants-1989_10
特許番号
US04873335

反応ノート

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