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Ammonia → 6-Fluoroquinazolin-4-ol

HRID 273777
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HRID 273777 반응식
[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]
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참가 물질

4

반응물 2

HCID 222AmmoniaHCID 200941616-Fluoro-2H-1,3-benzoxazine-2,4(3H)-dione

생성물 1

HCID 1354805206-Fluoroquinazolin-4-ol

시약·촉매·용매 1

HCID 713Formamide용매

실험 절차

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.

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후처리

  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

출처 및 근거

ORD 기록
ord-c8ade91d1bb14dda9d2126ec2d97e8f2
출처 데이터셋
uspto-grants-1995_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05387585

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