Trifluoromethanesulfonic acid → HCID 13920595, 화합물

HRID 569205노트

반응식

HRID 569205 반응식
[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

참가 물질

3

반응물 2

HCID 62406Trifluoromethanesulfonic acidHCID 20148818HCID 20148818, 화합물

생성물 1

HCID 13920595HCID 13920595, 화합물수율 38%

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-189722dad6644dd8a6ab93610b5cf63d
출처 데이터셋
uspto-grants-1988_03
특허 번호
US04731447

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