4-Ethylaniline → HCID 13121221, 화합물

HRID 544386노트

반응식

HRID 544386 반응식
Cl[C:2]1[C:7]([CH3:8])=[C:6]([CH3:9])[N:5]=[CH:4][N:3]=1.[CH2:10]([C:12]1[CH:18]=[CH:17][C:15]([NH2:16])=[CH:14][CH:13]=1)[CH3:11]>>[CH2:10]([C:12]1[CH:18]=[CH:17][C:15]([NH:16][C:2]2[C:7]([CH3:8])=[C:6]([CH3:9])[N:5]=[CH:4][N:3]=2)=[CH:14][CH:13]=1)[CH3:11]

참가 물질

3

반응물 2

HCID 115044-EthylanilineHCID 126003894-Chloro-5,6-dimethylpyrimidine

생성물 1

HCID 13121221HCID 13121221, 화합물수율 71%

반응 조건

온도
150 °C

실험 절차

To 4.3 g (0.03 mole) of 4-chloro-5,6-dimethylpyrimidine were added 3.6 g (0.03 mole) of p-ethylaniline; the mixture was then heated at 150° C. for about 3 minutes. The reaction mixture quickly became a solution which, on cooling, precipitated crystals. These crystals were separated and then made alkaline by the addition of 50 ml of a dilute aqueous solution of sodium hydroxide. The insolubles were extracted with about 100ml of ethyl acetate and the resulting extract was washed, in turn, with water and with a saturated aqueous solution of sodium chloride; it was then dried over anhydrous sodium sulphate. The ethyl acetate was distilledoff under reduced pressure to give crystals, which were recrystallised frombenzene, affording 4.8 g (yield 71%) of the desired Compound No. 46, in theform of colourless needles melting at 97°-98° C.

후처리

  1. temperatureon cooling
  2. customprecipitated crystals
  3. customThese crystals were separated
  4. additionby the addition of 50 ml of a dilute aqueous solution of sodium hydroxide
  5. extractionThe insolubles were extracted with about 100ml of ethyl acetate
  6. extractionthe resulting extract
  7. washwas washed, in turn, with water and with a saturated aqueous solution of sodium chloride
  8. dry with materialit was then dried over anhydrous sodium sulphate
  9. customto give crystals, which
  10. customwere recrystallised frombenzene,

출처 및 근거

ORD 기록
ord-a2457d24529e4e5f9307dcd7e305128a
출처 데이터셋
uspto-grants-1984_05
특허 번호
US04450162

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