Sodium 3-nitrobenzenesulfonate → N,N-Dimethyl-N-(2-benzoylaminoethyl)benzylammonium m-Nitrobenzenesulfonate

HRID 372940

반응식

HRID 372940 반응식
[N+:1]([C:4]1[CH:5]=[C:6]([S:10]([O-:13])(=[O:12])=[O:11])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[Na+].[Cl-].[CH3:16][N+:17]([CH2:30][C:31]1[CH:36]=[CH:35][CH:34]=[CH:33][CH:32]=1)([CH3:29])[CH2:18][CH2:19][NH:20][C:21](=[O:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1>O>[N+:1]([C:4]1[CH:5]=[C:6]([S:10]([O-:13])(=[O:11])=[O:12])[CH:7]=[CH:8][CH:9]=1)([O-:3])=[O:2].[CH3:29][N+:17]([CH2:30][C:31]1[CH:32]=[CH:33][CH:34]=[CH:35][CH:36]=1)([CH3:16])[CH2:18][CH2:19][NH:20][C:21](=[O:28])[C:22]1[CH:27]=[CH:26][CH:25]=[CH:24][CH:23]=1

참가 물질

4

반응물 2

HCID 31389Sodium 3-nitrobenzenesulfonateHCID 19811098N,N-Dimethyl-N-(2-benzoylaminoethyl)benzylammonium Chloride

생성물 1

HCID 86746309N,N-Dimethyl-N-(2-benzoylaminoethyl)benzylammonium m-Nitrobenzenesulfonate

시약·촉매·용매 1

HCID 962Water용매2회

실험 절차

A solution of 11.26 grams (0.05 mol) of sodium m-nitrobenzenesulfonate in 50 milliters of water was added to a solution of 15.94 grams (0.05 mol) of the N,N-dimethyl-N-(2-benzoylaminoethyl)benzylammonium chloride, prepared as described in Example 2, in 50 milliters of water. An oily precipitate formed. The water layer was decanted and the oil was rinsed with water, dissolved in methylene chloride, dried over magnesium sulfate and concentrated to a viscous oil. The oil was treated with ligroine (bp=35°-60° C.) with warming. The oil crystallized and the solid formed was collected and recrystallized from isopropanol. The yield of product was 10.75 grams (44.28% of theory); mp=109°-112° C.

후처리

  1. customprepared
  2. customAn oily precipitate formed
  3. customThe water layer was decanted
  4. washthe oil was rinsed with water
  5. dissolutiondissolved in methylene chloride
  6. dry with materialdried over magnesium sulfate
  7. concentrationconcentrated to a viscous oil
  8. additionThe oil was treated with ligroine (bp=35°-60° C.)
  9. temperaturewith warming
  10. customThe oil crystallized
  11. customthe solid formed
  12. customwas collected
  13. customrecrystallized from isopropanol

출처 및 근거

ORD 기록
ord-1306be5017d14878b275a1dd2041354e
출처 데이터셋
uspto-grants-1992_11
특허 번호
US05162188

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