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Sodium Hydroxide → 10-(p-fluoro-phenyl)-2,3-dihydro-imidazo[2,1-b]quinazolin-5(10H)-one

HRID 918197
ノート
印刷プレビュー

反応式

HRID 918197 の反応式
[F:1][C:2]1[CH:7]=[CH:6][C:5]([N:8]2[C:14](=O)[O:13][C:11](=O)[C:10]3=[CH:16][CH:17]=[CH:18][CH:19]=[C:9]23)=[CH:4][CH:3]=1.CSC1[NH:23][CH2:24][CH2:25][N:26]=1.[OH-].[Na+]>O1CCOCC1>[F:1][C:2]1[CH:3]=[CH:4][C:5]([N:8]2[C:9]3[C:10](=[CH:16][CH:17]=[CH:18][CH:19]=3)[C:11](=[O:13])[N:23]3[CH2:24][CH2:25][N:26]=[C:14]23)=[CH:6][CH:7]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 14798Sodium HydroxideHCID 883692-Methylthio-2-imidazoline hydroiodideHCID 12226008HCID 12226008、化合物

生成物 1

HCID 306383910-(p-fluoro-phenyl)-2,3-dihydro-imidazo[2,1-b]quinazolin-5(10H)-one

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

A solution of 5.4 g. of N-(p-fluoro-phenyl)isatoic anhydride, 2.5 g. of 2-methylmercapto-imidazoline and one pellet (about 100 mg.) sodium hydroxide in 75 ml. of dioxane is refluxed with stirring for 4 hours. The resulting mixture is evaporated to dryness, the residue dissolved in methylene chloride, washed with water and extracted twice with 1N hydrochloric acid. The combined aqueous extracts are washed with methylene chloride and then with diethyl ether and made basic with sodium bicarbonate. The resulting precipitate is filtered off, washed thoroughly with water, dried by suction, dissolved in methylene chloride, dried with sodium sulfate, treated with charcoal and the methylene chloride exchanged for methanol to crystallize 10-(p-fluoro-phenyl)-2,3-dihydro-imidazo[2,1-b]quinazolin-5(10H)-one, m.p. 278°-280°C.

後処理

  1. customThe resulting mixture is evaporated to dryness
  2. dissolutionthe residue dissolved in methylene chloride
  3. washwashed with water
  4. extractionextracted twice with 1N hydrochloric acid
  5. washThe combined aqueous extracts are washed with methylene chloride
  6. filtrationThe resulting precipitate is filtered off
  7. washwashed thoroughly with water
  8. customdried by suction
  9. dissolutiondissolved in methylene chloride
  10. dry with materialdried with sodium sulfate
  11. additiontreated with charcoal
  12. customto crystallize 10-(p-fluoro-phenyl)-2,3-dihydro-imidazo[2,1-b]quinazolin-5(10H)-one, m.p. 278°-280°C.

出典と根拠

ORDレコード
ord-e6524af921ba466e8234585c63884b08
出典データセット
uspto-grants-1976_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US03969506

反応ノート

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