Ammonia → 2-Amino-4,6-difluoropyrimidine

HRID 1085882노트

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HRID 1085882 반응식
[NH3:1].F[C:3]1[N:8]=[C:7]([F:9])[CH:6]=[C:5]([F:10])[N:4]=1>C(OCC)C>[NH2:1][C:3]1[N:8]=[C:7]([F:9])[CH:6]=[C:5]([F:10])[N:4]=1

참가 물질

4

반응물 2

HCID 222AmmoniaHCID 696772,4,6-Trifluoropyrimidine

생성물 1

HCID 12014802-Amino-4,6-difluoropyrimidine

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

반응 조건

온도
25 °C

실험 절차

69.7 g (4.1 mol) of liquid ammonia were added at -30° to -20° C. to a stirred mixture of 250 g (1.865 mol) of 2,4,6-trifluoropyrimidine and 3.3 1 of diethyl ether within 1 hour. To work up, the reaction mixture was warmed to 25° C. and the precipitate was filtered off. Washing with ether, stirring in water, renewed filtration and drying resulted in 203 g (83% of theory) of the desired product (melting point 214°-216° C.). It was possible by concentrating the ether filtrate to about 1/3 of its volume to isolate a further 20 g (8% of theory) of this compound, of melting point 193°-196° C., from a 1:1 mixture with the isomeric 4-amino compound. Comparative experiment (according to SU-A 547,447--1975)

후처리

  1. filtrationthe precipitate was filtered off
  2. washWashing with ether
  3. filtrationfiltration
  4. customdrying

출처 및 근거

ORD 기록
ord-724dbf67b047439b9a8f67d2e9ce2ad2
출처 데이터셋
uspto-grants-1991_04
특허 번호
US05011927

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