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

HRID 1197411
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반응식

HRID 1197411 반응식
[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
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참가 물질

4

반응물 2

HCID 222AmmoniaHCID 150227122,4-Difluoro-6-trifluoromethoxypyrimidine

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
-70 °C

실험 절차

At -75° to -70° C. and over a period of 1 hour, 8.7 g (0.51 mol) of gaseous ammonia was gassed, while stirring, into a mixture of 51 g (0.255 mol) of 2,4-difluoro-6-trifluoromethoxypyrimidine in 200 ml of diethyl ether. The mixture was stirred for 1 1/2 hours at -70° C. and for 1 hour at room temperature. The reaction mixture was evaporated down under reduced pressure, taken up in methylene chloride and extracted with water. The organic phase was dried, evaporated down and chromatographed over silica gel (8:1 ligroin/ether mixture) to give 38.1 g (75.6% of theory) of the title compound as colorless crystals of melting point 86°-89° C.

후처리

  1. customThe reaction mixture was evaporated down under reduced pressure
  2. extractionextracted with water
  3. customThe organic phase was dried
  4. customevaporated down
  5. customchromatographed over silica gel (8:1 ligroin/ether mixture)

출처 및 근거

ORD 기록
ord-552ebd0b3ea642679ece40248e32c2a2
출처 데이터셋
uspto-grants-1994_01
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05276007

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