N-Methylaniline → 2,4-Bis(N-methylphenylamino)thieno(2,3-d)pyrimidine

HRID 1198117노트

반응식

HRID 1198117 반응식
Cl[C:2]1[N:3]=[C:4](Cl)[C:5]2[CH:10]=[CH:9][S:8][C:6]=2[N:7]=1.[CH3:12][NH:13][C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1>C(Cl)(Cl)Cl>[CH3:12][N:13]([C:14]1[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1)[C:2]1[N:3]=[C:4]([N:13]([C:14]2[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=2)[CH3:12])[C:5]2[CH:10]=[CH:9][S:8][C:6]=2[N:7]=1

참가 물질

4

반응물 2

HCID 7515N-MethylanilineHCID 122173242,4-Dichlorothieno[2,3-d]pyrimidine

생성물 1

HCID 103156292,4-Bis(N-methylphenylamino)thieno(2,3-d)pyrimidine

시약·촉매·용매 1

HCID 6212Chloroform용매

실험 절차

2,4-Dichlorothieno[2,3-d]pyrimidine (2 g, 0.00975 mol) and N-methylaniline (5 ml) were heated in an oil bath at 150° for 2 hours. The reaction mixture was dissolved in chloroform (200 ml) and extracted with 2N hydrochloric acid (3×100 ml). The chloroform solution was then washed with sodium carbonate solution, dried over magnesium sulphate, filtered and evaporated to give an oil. The oil was purified by chromatography using dichloromethane as eluant. The solid obtained was recrystallized from ether/petroleum ether (b.p. 40°-60°) to give the title compound, (1.2 g) m.p. 85°-87°.

후처리

  1. extractionextracted with 2N hydrochloric acid (3×100 ml)
  2. washThe chloroform solution was then washed with sodium carbonate solution
  3. dry with materialdried over magnesium sulphate
  4. filtrationfiltered
  5. customevaporated
  6. customto give an oil
  7. customThe oil was purified by chromatography
  8. customThe solid obtained
  9. customwas recrystallized from ether/petroleum ether (b.p. 40°-60°)

출처 및 근거

ORD 기록
ord-feea85f7879d4eb4abbffa364b47048a
출처 데이터셋
uspto-grants-1994_01
특허 번호
US05280026

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