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

HRID 414795

反応式

HRID 414795 の反応式
[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]

参加物

5

反応物 3

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-d6e50eb0df8941a9b773da1001eb169d
出典データセット
uspto-grants-1988_12
特許番号
US04794186

関連ノート

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