HCID 20188328、化合物 → (+/-)-1-[2-Hydroxy-2-[4-((methylsulfonyl)amino)phenyl]ethyl]-3-methyl-1H-imidazolium chloride

HRID 65254ノート

反応式

HRID 65254 の反応式
[ClH:1].[N+](C1C=CC(CCC[CH2:14][N:15]2[CH:19]=[CH:18][N:17]=[CH:16]2)=CC=1)([O-])=O.[Cl-].[CH3:21][S:22]([NH:25][C:26]1[CH:31]=[CH:30][C:29]([C:32](=[O:39])[CH2:33]C2[NH2+]C=CN=2)=[CH:28][CH:27]=1)(=[O:24])=[O:23]>O.[Pd]>[Cl-:1].[OH:39][CH:32]([C:29]1[CH:28]=[CH:27][C:26]([NH:25][S:22]([CH3:21])(=[O:23])=[O:24])=[CH:31][CH:30]=1)[CH2:33][NH+:17]1[CH:18]=[CH:19][N:15]([CH3:14])[CH2:16]1

参加物

5

反応物 2

HCID 20188328HCID 20188328、化合物HCID 86741032HCID 86741032、化合物

生成物 1

HCID 20188316(+/-)-1-[2-Hydroxy-2-[4-((methylsulfonyl)amino)phenyl]ethyl]-3-methyl-1H-imidazolium chloride

試薬・触媒・溶媒 2

HCID 23938Palladium触媒HCID 962Water溶媒

実験手順

A solution of 152.3 g (0.463 mole) of 3-methyl-1[2-[4-((methylsulfonyl)amino)phenyl-2-oxoethyl]-1H-imidazolium chloride in 1 L of distilled water and 7.62 g 10% Pd/C catalyst are placed in a 2 L Parr bottle and hydrogenated at 50 psi pressure for ca. 5 hours. Additional H2 is added as needed to maintain 50 psi pressure. The reaction mixture is filtered and the solvent is evaporated by azeotroping with ethanol to provide the title compound, which may be recrystallized from aqueous ethanol.

後処理

  1. additionAdditional H2 is added
  2. temperatureto maintain 50 psi pressure
  3. filtrationThe reaction mixture is filtered
  4. customthe solvent is evaporated
  5. customby azeotroping with ethanol

出典と根拠

ORDレコード
ord-06859232194a438e81b6a8cfaddc161c
出典データセット
uspto-grants-1986_09
特許番号
US04613609

反応ノート

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