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

HRID 1198117ノート

反応式

HRID 1198117 の反応式
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

参加物

4

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

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°.

後処理

  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°)

出典と根拠

ORDレコード
ord-feea85f7879d4eb4abbffa364b47048a
出典データセット
uspto-grants-1994_01
特許番号
US05280026

反応ノート

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