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Ammonia → 6-Fluoroquinazolin-4-ol

HRID 273777
ノート
印刷プレビュー

反応式

HRID 273777 の反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]2O[C:9](=O)[NH:8][C:7](=[O:12])[C:6]=2[CH:13]=1.[NH3:14]>C(N)=O>[F:1][C:2]1[CH:13]=[C:6]2[C:5](=[CH:4][CH:3]=1)[N:14]=[CH:9][NH:8][C:7]2=[O:12]
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 222AmmoniaHCID 200941616-Fluoro-2H-1,3-benzoxazine-2,4(3H)-dione

生成物 1

HCID 1354805206-Fluoroquinazolin-4-ol

試薬・触媒・溶媒 1

HCID 713Formamide溶媒

実験手順

1. 3.62 g of 6-fluoro-2H-1,3-benzoxazine-2,4(1H)-dione are suspended in 15 ml of formamide. Gaseous ammonia is introduced while stirring during about 10 min. until the suspension is saturated and the mixture is stirred at room temperature for a further 1 h. Subsequently, the mixture is stirred at 125° C. (bath temperature) for 16 h. The solvent is then distilled off in a high vacuum. The residue is triturated in 50 ml of water and then cooled slightly. The resulting crystals are filtered off, washed with ice-cold water and dried over calcium chloride in a vacuum. 2.9 g of crude 6-fluoro-3H-quinazoline-4-one are obtained. The substance melts at 252°-255° C. after recrystallization from ethyl acetate.

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

後処理

  1. stirringthe mixture is stirred at room temperature for a further 1 h
  2. stirringSubsequently, the mixture is stirred at 125° C. (bath temperature) for 16 h
  3. distillationThe solvent is then distilled off in a high vacuum
  4. customThe residue is triturated in 50 ml of water
  5. temperaturecooled slightly
  6. filtrationThe resulting crystals are filtered off
  7. washwashed with ice-cold water
  8. dry with materialdried over calcium chloride in a vacuum

出典と根拠

ORDレコード
ord-c8ade91d1bb14dda9d2126ec2d97e8f2
出典データセット
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05387585

反応ノート

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