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Water → HCID 178438403、化合物

HRID 2260041
ノート
印刷プレビュー

反応式

HRID 2260041 の反応式
[CH2:1]([C:4]1[NH:8][N:7]=[C:6]([NH:9][C:10](=[N:12]O)[CH3:11])[CH:5]=1)[CH2:2][CH3:3].N1C=CC=CC=1.C1(C)C=CC(S(Cl)(=O)=O)=CC=1.O>CN(C)C(=O)C>[CH3:11][C:10]1[NH:9][C:6]2[N:7]([N:8]=[C:4]([CH2:1][CH2:2][CH3:3])[CH:5]=2)[N:12]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 962WaterHCID 1049PyridineHCID 73974-Toluenesulfonyl chlorideHCID 178439388HCID 178439388、化合物

生成物 1

HCID 178438403HCID 178438403、化合物

試薬・触媒・溶媒 1

HCID 31374Dimethylacetamide溶媒

実験手順

A 5.38 g portion of N-(5-propyl-1H-pyrazol-3-yl)acetamidoxime was dissolved in 45 ml of N,N-dimethylacetamide. With cooling on an ice bath, to this were added 2.39 ml of pyridine and 5.63 g of p-toluenesulfonic acid chloride, followed by 30 minutes of stirring at the same temperature and additional 3 hours of stirring at room temperature. The resulting reaction mixture was added to 350 ml of water and extracted with chloroform. After distilling off chloroform from the organic layer under a reduced pressure, the thus obtained residue was dissolved in 135 ml of methanol, mixed with 2.39 ml of pyridine and then heated under reflux for 2 hours.

後処理

  1. temperatureWith cooling on an ice bath
  2. stirringof stirring at room temperature
  3. customThe resulting reaction mixture
  4. extractionextracted with chloroform
  5. distillationAfter distilling off chloroform from the organic layer under a reduced pressure
  6. dissolutionthe thus obtained residue was dissolved in 135 ml of methanol
  7. additionmixed with 2.39 ml of pyridine
  8. temperatureheated
  9. temperatureunder reflux for 2 hours

出典と根拠

ORDレコード
ord-6e1ac42171a44cb1baf37efc7ed56d9a
出典データセット
uspto-grants-1995_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05475114

反応ノート

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