Ammonia → 2-Amino-4,6-difluoropyrimidine

HRID 1085882ノート

反応式

HRID 1085882 の反応式
[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

参加物

4

反応物 2

HCID 222AmmoniaHCID 696772,4,6-Trifluoropyrimidine

生成物 1

HCID 12014802-Amino-4,6-difluoropyrimidine

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
25 °C

実験手順

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)

後処理

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

出典と根拠

ORDレコード
ord-724dbf67b047439b9a8f67d2e9ce2ad2
出典データセット
uspto-grants-1991_04
特許番号
US05011927

反応ノート

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