Methyl Methanesulfonate → 1-Methyl-3-[3-[4-(5-trifluoromethyl-1,2,4-oxadiazol-3-yl)-2,6-dimethylphenoxy]-propyl]-pyridinium methanesulfonate

HRID 963319

반응식

HRID 963319 반응식
[F:1][C:2]([F:27])([F:26])[C:3]1[O:7][N:6]=[C:5]([C:8]2[CH:23]=[C:22]([CH3:24])[C:11]([O:12][CH2:13][CH2:14][CH2:15][C:16]3[CH:17]=[N:18][CH:19]=[CH:20][CH:21]=3)=[C:10]([CH3:25])[CH:9]=2)[N:4]=1.[CH3:28][S:29]([O:32]C)(=[O:31])=[O:30]>C(Cl)Cl>[CH3:28][S:29]([O-:32])(=[O:31])=[O:30].[CH3:28][N+:18]1[CH:19]=[CH:20][CH:21]=[C:16]([CH2:15][CH2:14][CH2:13][O:12][C:11]2[C:22]([CH3:24])=[CH:23][C:8]([C:5]3[N:4]=[C:3]([C:2]([F:1])([F:26])[F:27])[O:7][N:6]=3)=[CH:9][C:10]=2[CH3:25])[CH:17]=1

참가 물질

4

반응물 2

HCID 4156Methyl Methanesulfonate2회HCID 190820123-[3-[4-(5-Trifluoromethyl-1,2,4-oxadiazol-3-yl)-2,6-dimethylphenoxy]-propyl]-pyridine

생성물 1

HCID 190820401-Methyl-3-[3-[4-(5-trifluoromethyl-1,2,4-oxadiazol-3-yl)-2,6-dimethylphenoxy]-propyl]-pyridinium methanesulfonate수율 157%

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

To a solution of 3-[3-[4-(5-trifluoromethyl-1,2,4-oxadiazol-3-yl)-2,6-dimethylphenoxy]-propyl]-pyridine (1 g, 2.6 mmol, 1.1 eq) in 10 ml of methylene chloride was added methyl methanesulfonate (0.32 g, 2.9 mmol) and the mixture was gently refluxed overnight. After adding 0.5 eq of methyl methanesulfonate, the mixture was allowed to reflux an additional 24 h. The mixture was concentrated in vacuo and a solid residue was washed with ether to afford 1.11 g (85.3%) of 1-methyl-3-[3-[4-(5-trifluoromethyl-1,2,4-oxadiazol-3-yl)-2,6-dimethylphenoxy]-propyl]-pyridinium methanesulfonate, as a white powder.

후처리

  1. temperatureto reflux an additional 24 h
  2. concentrationThe mixture was concentrated in vacuo
  3. washa solid residue was washed with ether

출처 및 근거

ORD 기록
ord-be7cb0573eb543ca967f7964071715cc
출처 데이터셋
uspto-grants-1998_06
특허 번호
US05763461

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