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

HRID 53214

反応式

HRID 53214 の反応式
[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

参加物

4

反応物 2

HCID 4156Methyl Methanesulfonate2 回HCID 190820123-[3-[4-(5-Trifluoromethyl-1,2,4-oxadiazol-3-yl)-2,6-dimethylphenoxy]-propyl]-pyridine

生成物 1

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

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

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

出典と根拠

ORDレコード
ord-4137d816472d4cdeb63c64978c7718ac
出典データセット
uspto-grants-1997_04
特許番号
US05618821

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