N,N-Dimethylaniline → ethyl (2Z)-2-(2-acetamido-1,3-thiazol-4-yl)-2-(2-oxopyrrolidin-3-yl)oxyiminoacetate

HRID 414795

반응식

HRID 414795 반응식
[NH:1]1[CH2:5][CH2:4][CH:3]([O:6]/[N:7]=[C:8](/[C:14](=O)[CH2:15]Cl)\[C:9]([O:11][CH2:12][CH3:13])=[O:10])[C:2]1=[O:18].[C:19]([NH:22][C:23]([NH2:25])=[S:24])(=[O:21])[CH3:20].CN(C)C1C=CC=CC=1>C(O)C>[C:19]([NH:22][C:23]1[S:24][CH:15]=[C:14](/[C:8](=[N:7]/[O:6][CH:3]2[CH2:4][CH2:5][NH:1][C:2]2=[O:18])/[C:9]([O:11][CH2:12][CH3:13])=[O:10])[N:25]=1)(=[O:21])[CH3:20]

참가 물질

5

반응물 3

HCID 949N,N-DimethylanilineHCID 2723593AcetylthioureaHCID 13536861ethyl (2Z)-4-chloro-3-oxo-2-(2-oxopyrrolidin-3-yl)oxyiminobutanoate

생성물 1

HCID 13536846ethyl (2Z)-2-(2-acetamido-1,3-thiazol-4-yl)-2-(2-oxopyrrolidin-3-yl)oxyiminoacetate수율 49.9%

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

2.77 g of ethyl (Z)-2-[(2-pyrrolidon-3-yl)oxyimino]-3-oxo-4-chloro-n-butyrate and 1.2 g of acetylthiourea are added to 20 ml of ethanol, and 2.0 g of N,N-dimethylaniline are added thereto. The mixture is stirred at 20° to 30° C. for 4 hours. Then, the mixture is concentrated under reduced pressure to drynss. The residue is dissolved in chloroform, and the solution is washed with water and an aqueous sodium bicarbonate solution, successively. The chloroform solution is dried and concentrated under reduced pressure to remove solvent. The residue is crystallized with isopropanol, and the crystals are collected by filtration. 1.7 g of ethyl (Z)-2-(2-acetamidothiazol-4-yl)-2-[(2-pyrrolidon-3-yl)oxyimino]acetate are obtained.

후처리

  1. additionare added
  2. concentrationThen, the mixture is concentrated under reduced pressure
  3. dissolutionThe residue is dissolved in chloroform
  4. washthe solution is washed with water
  5. dry with materialThe chloroform solution is dried
  6. concentrationconcentrated under reduced pressure
  7. customto remove solvent
  8. customThe residue is crystallized with isopropanol
  9. filtrationthe crystals are collected by filtration

출처 및 근거

ORD 기록
ord-d6e50eb0df8941a9b773da1001eb169d
출처 데이터셋
uspto-grants-1988_12
특허 번호
US04794186

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