Ammonia → HCID 19874089, 화합물

HRID 465360노트

반응식

HRID 465360 반응식
[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

참가 물질

6

반응물 4

HCID 222AmmoniaHCID 313Hydrochloric AcidHCID 97423-FluoroanilineHCID 19804698HCID 19804698, 화합물

생성물 1

HCID 19874089HCID 19874089, 화합물

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

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).

후처리

  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)

출처 및 근거

ORD 기록
ord-46505254dfd144619a2accecd0417b5d
출처 데이터셋
uspto-grants-1992_10
특허 번호
US05153200

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