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Ammonia → 2-Amino-4-fluoro-6-trifluoromethoxypyrimidine

HRID 232518
ノート
印刷プレビュー

反応式

HRID 232518 の反応式
[NH3:1].F[C:3]1[N:8]=[C:7]([F:9])[CH:6]=[C:5]([O:10][C:11]([F:14])([F:13])[F:12])[N:4]=1>C(OCC)C>[NH2:1][C:3]1[N:8]=[C:7]([F:9])[CH:6]=[C:5]([O:10][C:11]([F:14])([F:13])[F:12])[N:4]=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 222AmmoniaHCID 150227122,4-Difluoro-6-trifluoromethoxypyrimidine

生成物 1

HCID 150227162-Amino-4-fluoro-6-trifluoromethoxypyrimidine

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

8.7 g (0.51 mol) of gaseous ammonia were passed into a mixture of 51 g (0.255 mol) of 2,4-difluoro-6-trifluoromethoxypyrimidine in 200 ml of diethyl ether in the course of 1 hour at from -75° to -70° C. while stirring. Stirring was continued for a further 11/2 hours at -70° C. and for 1 hour at room temperature. The reaction mixture was evaporated down under reduced pressure, the residue was taken up in methylene chloride and the solution was extracted with water. After the organic phase had been dried, evaporated down and chromatographed over silica gel using 8:1 petroleum ether/ether, 38.1 g (75.6% of theory) of the title compound were obtained as colorless crystals of melting point 86°-89° C.

後処理

  1. stirringStirring
  2. custom2 hours
  3. customat -70° C.
  4. customThe reaction mixture was evaporated down under reduced pressure
  5. extractionthe solution was extracted with water
  6. customAfter the organic phase had been dried
  7. customevaporated down
  8. customchromatographed over silica gel using 8:1 petroleum ether/ether, 38.1 g (75.6% of theory) of the title compound
  9. customwere obtained as colorless crystals of melting point 86°-89° C.

出典と根拠

ORDレコード
ord-bff6f921969442869d097fe364d5a0a4
出典データセット
uspto-grants-1997_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05591694

反応ノート

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