Sodium Sulfate → 2-Hydroxyimino-N-{4-[2-(2-oxo-oxazolidin-3-yl)ethyl]phenyl}acetamide

HRID 241748

반응식

HRID 241748 반응식
S([O-])([O-])(=O)=O.[Na+].[Na+].[OH2:8].Cl[C:10](Cl)(Cl)[CH:11]=[O:12].[NH2:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][N:24]2[CH2:28][CH2:27][O:26][C:25]2=[O:29])=[CH:18][CH:17]=1.Cl.[NH2:31]O>O.Cl>[OH:8][N:31]=[CH:10][C:11]([NH:15][C:16]1[CH:21]=[CH:20][C:19]([CH2:22][CH2:23][N:24]2[CH2:28][CH2:27][O:26][C:25]2=[O:29])=[CH:18][CH:17]=1)=[O:12]

참가 물질

7

반응물 4

HCID 24436Sodium SulfateHCID 443297Hydroxyamine hydrochlorideHCID 107034763-(2-(4-Aminophenyl)ethyl)-1,3-oxazolidin-2-oneHCID 205283762,2,2-Trichloroacetaldehyde hydrate

생성물 1

HCID 866624332-Hydroxyimino-N-{4-[2-(2-oxo-oxazolidin-3-yl)ethyl]phenyl}acetamide

시약·촉매·용매 2

HCID 313Hydrochloric Acid용매HCID 962Water용매3회

실험 절차

Sodium sulphate (78.3 g) is added to a solution of trichloroacetaldehyde hydrate (32.5 mmoles) in water (100 ml). To the resulting suspension there are added a solution of 3-[2-(4-amino-phenyl)ethyl]oxazolidin-2-one in water (20 ml) and concentrated HCl solution (2.83 ml). A solution of hydroxylamine hydrochloride (95 mmoles) in water (50 ml) is then added. The reaction mixture is heated at reflux for two hours. The mixture is then cooled to ambient temperature. The solid formed is then filtered off, washed with water and dried in vacuo in the presence of P2O5 and at 40° C. overnight to yield the title product, which is used directly in the next Step.

후처리

  1. temperatureThe reaction mixture is heated
  2. temperatureat reflux for two hours
  3. customThe solid formed
  4. filtrationis then filtered off
  5. washwashed with water
  6. dry with materialdried in vacuo in the presence of P2O5 and at 40° C. overnight

출처 및 근거

ORD 기록
ord-64e59fa5f1e24f38bf1b501021197d01
출처 데이터셋
uspto-grants-2014_02
특허 번호
US08653073B2

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