o-Toluenesulfonyl chloride → HCID 22099729, 화합물

HRID 1457647노트

반응식

HRID 1457647 반응식
[CH2:1]([O:3][C:4](=[O:19])[CH2:5][CH2:6][CH2:7][NH:8][C:9]1[CH:18]=[CH:17][CH:16]=[CH:15][C:10]=1[C:11]([O:13][CH3:14])=[O:12])[CH3:2].[CH3:20][C:21]1[CH:26]=[CH:25][CH:24]=[CH:23][C:22]=1[S:27](Cl)(=[O:29])=[O:28]>N1C=CC=CC=1>[CH2:1]([O:3][C:4](=[O:19])[CH2:5][CH2:6][CH2:7][N:8]([C:9]1[CH:18]=[CH:17][CH:16]=[CH:15][C:10]=1[C:11]([O:13][CH3:14])=[O:12])[S:27]([C:22]1[CH:23]=[CH:24][CH:25]=[CH:26][C:21]=1[CH3:20])(=[O:29])=[O:28])[CH3:2]

참가 물질

4

반응물 2

HCID 8623o-Toluenesulfonyl chlorideHCID 266836Methyl 2-[(4-ethoxy-4-oxobutyl)amino]benzoate

생성물 1

HCID 22099729HCID 22099729, 화합물수율 90.7%

시약·촉매·용매 1

HCID 1049Pyridine용매

실험 절차

A mixture of 2.65 g of methyl 2-[(4-ethoxy-4-oxobutyl)amino]benzoate, 2.0 g of 2-methylphenylsulfonyl chloride and pyridine is heated on a steam bath for 16 hours. The mixture is concentrated under a vacuum (remove pyridine) and 1N HCl added. The mixture is extracted with dichloromethane and the extract washed with 1NHCl, H2O, 1M NaHCO3, brine and dried (Na2SO4). The solution is filtered through a thin pad of hydrons magnesium silicate and the filtrate evaporated to give 3.8 g of solid which is crystallized from ethanol to give crystals, m.p. 100°-102° C.

후처리

  1. temperatureis heated on a steam bath for 16 hours
  2. concentrationThe mixture is concentrated under a vacuum (remove pyridine) and 1N HCl
  3. additionadded
  4. extractionThe mixture is extracted with dichloromethane
  5. washthe extract washed with 1NHCl, H2O, 1M NaHCO3, brine
  6. dry with materialdried (Na2SO4)
  7. filtrationThe solution is filtered through a thin pad of hydrons magnesium silicate
  8. customthe filtrate evaporated

출처 및 근거

ORD 기록
ord-8fef0a5ed1474e2fb06b85677cec9daf
출처 데이터셋
uspto-grants-1998_12
특허 번호
US05849735

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