Ammonia → HCID 19874089、化合物

HRID 2106895ノート

反応式

HRID 2106895 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][CH:8]=1)[NH2:5].Cl[C:10]1[N:15]=[C:14]([CH3:16])[CH:13]=[C:12]([CH:17]2[CH2:19][CH2:18]2)[N:11]=1.Cl.N>C(O)C>[F:1][C:2]1[CH:3]=[C:4]([NH:5][C:10]2[N:15]=[C:14]([CH3:16])[CH:13]=[C:12]([CH:17]3[CH2:19][CH2:18]3)[N:11]=2)[CH:6]=[CH:7][CH:8]=1

参加物

6

反応物 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 97423-FluoroanilineHCID 19804698HCID 19804698、化合物

生成物 1

HCID 19874089HCID 19874089、化合物

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

A solution of 5.5 g (50 mmol) of 3-fluoroaniline and 9.3 g (55 mmol) of 2-chloro-4-methyl-6-cyclopropylpyrimidine in 100 ml of ethanol is adjusted to pH 1 with 5 ml of concentrated hydrochloric acid with stirring, and is then heated under reflux for 18 hours. After the brown emulsion has been cooled to room temperature, it is rendered alkaline with 10 ml of 30% ammonia, poured onto 100 ml of ice-water and extracted twice with 150 ml of diethyl ether each time. The combined extracts are washed with 50 ml of water, dried over sodium sulfate and filtered, and the solvent is evaporated. The yellowish crystals which remain are purified by recrystallisation from diisopropyl ether/petroleum ether (b.p. 50°-70° C.). The white crystals melt at 87°-89° C.; yield: 8.3 g (34 mmol; 68% of the theoretical yield).

後処理

  1. temperatureis then heated
  2. temperatureunder reflux for 18 hours
  3. extractionextracted twice with 150 ml of diethyl ether each time
  4. washThe combined extracts are washed with 50 ml of water
  5. dry with materialdried over sodium sulfate
  6. filtrationfiltered
  7. customthe solvent is evaporated
  8. customThe yellowish crystals which remain are purified by recrystallisation from diisopropyl ether/petroleum ether (b.p. 50°-70° C.)
  9. custommelt at 87°-89° C.
  10. custom68% of the theoretical yield)

出典と根拠

ORDレコード
ord-9d11f43d481642599c9561f75378b819
出典データセット
uspto-grants-1990_06
特許番号
US04931560

反応ノート

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