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Methanesulfonic Acid → 4-[4-(6-Chloro-2-naphthoyl)-1-piperidyl]-1-(4-fluorophenyl)-1-butanone methanesulfonate

HRID 1389877
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HRID 1389877 반응식
[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([C:12]([CH:14]1[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][CH2:22][C:23]([C:25]3[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=3)=[O:24])[CH2:16][CH2:15]1)=[O:13])[CH:6]=[CH:5]2.[CH3:32][S:33]([OH:36])(=[O:35])=[O:34]>C(#N)C>[CH3:32][S:33]([OH:36])(=[O:35])=[O:34].[Cl:1][C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][CH:11]=1)[CH:8]=[C:7]([C:12]([CH:14]1[CH2:19][CH2:18][N:17]([CH2:20][CH2:21][CH2:22][C:23]([C:25]3[CH:30]=[CH:29][C:28]([F:31])=[CH:27][CH:26]=3)=[O:24])[CH2:16][CH2:15]1)=[O:13])[CH:6]=[CH:5]2
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 6395Methanesulfonic AcidHCID 202956124-[4-(6-Chloro-2-naphthoyl)-1-piperidyl]-1-(4-fluorophenyl)-1-butanone

생성물 1

HCID 867374524-[4-(6-Chloro-2-naphthoyl)-1-piperidyl]-1-(4-fluorophenyl)-1-butanone methanesulfonate

시약·촉매·용매 1

HCID 6342Acetonitrile용매

실험 절차

The 4-[4-(6-chloro-2-naphthoyl)-1-piperidyl]-1-(4-fluorophenyl)-1-butanone prepared in Example 25 is dissolved in acetonitrile and 0.6 ml (9.2 mmoles) of methanesulfonic acid added. The mixture is stirred for 5 minutes and concentrated in vacuo and the residue stirred in anhydrous ether for 18 hours. The ether is decanted and the residue recrystallized from butanone and toluene to yield 4-[4-(6-chloro-2-naphthoyl)-1-piperidyl]-1-(4-fluorophenyl)-1-butanone methanesulfonate. M.P. 172°-5°.

후처리

  1. concentrationconcentrated in vacuo
  2. stirringthe residue stirred in anhydrous ether for 18 hours
  3. customThe ether is decanted
  4. customthe residue recrystallized from butanone and toluene

출처 및 근거

ORD 기록
ord-463e7ee597334b7f9e6549fc352cdc8f
출처 데이터셋
uspto-grants-1981_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US04246268

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