Methanol → HCID 178440127、化合物

HRID 1249554ノート

反応式

HRID 1249554 の反応式
[CH3:1][CH:2]([C:4]1[N:5]=[C:6]([C:17]([C:23]([F:26])([F:25])[F:24])([C:19]([F:22])([F:21])[F:20])[NH2:18])[NH:7][C:8]=1[C:9]1[CH:14]=[CH:13][C:12](SC)=[CH:11][CH:10]=1)[CH3:3].O[O:28][S:29]([O-:31])=O.[K+].S(OOS([O-])(=O)=O)(O)(=O)=O.[K+].[CH3:44]O>>[CH3:1][CH:2]([C:4]1[N:5]=[C:6]([C:17]([C:23]([F:26])([F:24])[F:25])([C:19]([F:20])([F:21])[F:22])[NH2:18])[NH:7][C:8]=1[C:9]1[CH:10]=[CH:11][C:12]([S:29]([CH3:44])(=[O:31])=[O:28])=[CH:13][CH:14]=1)[CH3:3]

参加物

5

反応物 4

HCID 887MethanolHCID 23690007Potassium hydrogen persulfateHCID 23707502Potassium hydroxy sulfiteHCID 178503126HCID 178503126、化合物

生成物 1

HCID 178440127HCID 178440127、化合物

実験手順

A mixture of 1.8 g (4.5 mmoles) of 4-(1-methylethyl)-5-(4-methylthiophenyl)-α,α-bis(trifluoromethyl)-1H-imidazole-2-methanamine, 7.25 g (11.8 mmoles) of Oxone® (potassium hydrogen persulfate) and 50 ml of methanol were stirred together overnight. The solid was filtered off and the filtrate was evaporated in vacuo. The residue was partitioned between ethyl acetate and water and the layers were separated. The organic layer was washed with water and brine, dried over anhydrous magnesium sulfate and concentrated in vacuo to afford 2.1 g of an oil. The product was purified via flash chromatography on silica gel (73:27 hexane/ethyl acetate) to afford 1.02 g (53%) of the title compound as an off-white crystalline solid, m.p. 155°-157° C.

後処理

  1. filtrationThe solid was filtered off
  2. customthe filtrate was evaporated in vacuo
  3. customThe residue was partitioned between ethyl acetate and water
  4. customthe layers were separated
  5. washThe organic layer was washed with water and brine
  6. dry with materialdried over anhydrous magnesium sulfate
  7. concentrationconcentrated in vacuo

出典と根拠

ORDレコード
ord-2ddad78127a04d1fa487356fe01948d8
出典データセット
uspto-grants-1986_12
特許番号
US04632930

反応ノート

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