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Potassium Hydroxide → HCID 58012168、化合物

HRID 660896
ノート
印刷プレビュー

反応式

HRID 660896 の反応式
C([O:3][C:4](=[O:22])[CH2:5][N:6]1[C:10](=[O:11])[N:9]([CH2:12][CH:13]=[CH2:14])[C:8]([C:15]2[CH:20]=[CH:19][C:18]([Cl:21])=[CH:17][CH:16]=2)=[N:7]1)C.[OH-].[K+]>CO>[Cl:21][C:18]1[CH:19]=[CH:20][C:15]([C:8]2[N:9]([CH2:12][CH:13]=[CH2:14])[C:10](=[O:11])[N:6]([CH2:5][C:4]([OH:22])=[O:3])[N:7]=2)=[CH:16][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 14797Potassium HydroxideHCID 86675482ethyl[3-(4-chlorophenyl)-4-allyl-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]-acetate

生成物 1

HCID 58012168HCID 58012168、化合物

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

4.88 g (15.9 mmol) of ethyl[3-(4-chlorophenyl)-4-allyl-5-oxo-4,5-dihydro-1H-1,2,4-triazol-1-yl]-acetate from Example 214A are placed in 48 ml methanol and stirred with 5 ml 20% aqueous potassium hydroxide for 2 hrs at room temperature. The solution is concentrated to ca. one half, then diluted with water and extracted with ethyl acetate. The aqueous phase is acidified with ca. 2 ml of conc. hydrochloric acid and extracted twice with 100 ml ethyl acetate each time. The last organic extracts are combined, dried over sodium sulphate, filtered and concentrated in vacuo. After drying in high vacuum, 4.20 g (90% of theory) of the target compound are thus obtained.

後処理

  1. concentrationThe solution is concentrated
  2. additiondiluted with water
  3. extractionextracted with ethyl acetate
  4. extractionextracted twice with 100 ml ethyl acetate each time
  5. dry with materialdried over sodium sulphate
  6. filtrationfiltered
  7. concentrationconcentrated in vacuo
  8. customAfter drying in high vacuum, 4.20 g (90% of theory) of the target compound
  9. customare thus obtained

出典と根拠

ORDレコード
ord-7f5a1a9e070e4e1f9ef3296b983f3ef5
出典データセット
uspto-grants-2011_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08084481B2

反応ノート

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このページの内容参加物実験手順後処理出典と根拠反応ノート