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1,4-Dioxane → Fluquazone

HRID 1395150
ノート
印刷プレビュー

反応式

HRID 1395150 の反応式
[F:1][C:2]([F:23])([F:22])[CH2:3][N:4]1[C:13]2[C:8](=[CH:9][C:10]([Cl:14])=[CH:11][CH:12]=2)[CH:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)[NH:6][C:5]1=S.[O:24]1CCOCC1.[K]>C(O)=O.O>[F:1][C:2]([F:23])([F:22])[CH2:3][N:4]1[C:13]2[C:8](=[CH:9][C:10]([Cl:14])=[CH:11][CH:12]=2)[C:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][CH:16]=2)=[N:6][C:5]1=[O:24]
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 3

HCID 312751,4-DioxaneHCID 5462222PotassiumHCID 203406541-(2,2,2-trifluoroethyl)-4-phenyl-6-chloro-3,4-dihydro-2(1H)-quinazolinethione

生成物 1

HCID 219069Fluquazone

試薬・触媒・溶媒 2

HCID 284Formic Acid触媒HCID 962Water溶媒

実験手順

To a solution of 1.5 g of 1-(2,2,2-trifluoroethyl)-4-phenyl-6-chloro-3,4-dihydro-2(1H)-quinazolinethione in 50 ml. of dioxane was added dropwise a solution of 3 g of potassium permangenate in 20 ml. of water. The mixture was stirred at room temperature for 2 hours and then a few drops of formic acid was added. The resultant brown precipitate was filtered off and washed with chloroform. The filtrate was concentrated under reduced pressure and the residue was dissolved in 30 ml. of chloroform. The chloroform solution was combined, washed successively with dilute sodium hydroxide solution and water, and dried over anhydrous sodium sulfate. The solvent was removed under reduced pressure. The residue was recrystallized from isopropyl alcohol to give 1 g of 1-(2,2,2-trifluoroethyl)-4-phenyl-6-chloro-2(1H)-quinazolinone, m.p. 184.0°-185.0° C.

後処理

  1. filtrationThe resultant brown precipitate was filtered off
  2. washwashed with chloroform
  3. concentrationThe filtrate was concentrated under reduced pressure
  4. dissolutionthe residue was dissolved in 30 ml
  5. washwashed successively with dilute sodium hydroxide solution and water
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was removed under reduced pressure
  8. customThe residue was recrystallized from isopropyl alcohol

出典と根拠

ORDレコード
ord-1804be5b322e4790a48a11bd6a4dc91e
出典データセット
uspto-grants-1980_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04202895

反応ノート

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