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

HRID 65254노트

반응식

HRID 65254 반응식
[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

참가 물질

5

반응물 2

HCID 20188328HCID 20188328, 화합물HCID 86741032HCID 86741032, 화합물

생성물 1

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

시약·촉매·용매 2

HCID 23938Palladium촉매HCID 962Water용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-06859232194a438e81b6a8cfaddc161c
출처 데이터셋
uspto-grants-1986_09
특허 번호
US04613609

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