Trifluoroacetic acid → 1-(2,6-Dichlorophenyl)-3-[6-methoxy-7-(6-methylamino-1-hexynyl)quinazolin-4-yl]urea

HRID 393246ノート

反応式

HRID 393246 の反応式
[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[NH:9][C:10]([NH:12][C:13]1[C:22]2[C:17](=[CH:18][C:19]([C:25]#[C:26][CH2:27][CH2:28][CH2:29][CH2:30][N:31](NC(OC(C)(C)C)=O)[CH3:32])=[C:20]([O:23][CH3:24])[CH:21]=2)[N:16]=[CH:15][N:14]=1)=[O:11].FC(F)(F)C(O)=O>C(Cl)Cl>[Cl:1][C:2]1[CH:7]=[CH:6][CH:5]=[C:4]([Cl:8])[C:3]=1[NH:9][C:10]([NH:12][C:13]1[C:22]2[C:17](=[CH:18][C:19]([C:25]#[C:26][CH2:27][CH2:28][CH2:29][CH2:30][NH:31][CH3:32])=[C:20]([O:23][CH3:24])[CH:21]=2)[N:16]=[CH:15][N:14]=1)=[O:11]

参加物

4

反応物 2

HCID 6422Trifluoroacetic acidHCID 226492701-(2,6-dichlorophenyl)-3-{7-[6-(N-tert-butoxycarbonylamino-N-methylamino)-1-hexynyl]-6-methoxyquinazolin-4-yl}urea

生成物 1

HCID 226493301-(2,6-Dichlorophenyl)-3-[6-methoxy-7-(6-methylamino-1-hexynyl)quinazolin-4-yl]urea

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

A mixture of 1-(2,6-dichlorophenyl)-3-{7-[6-(N-tert-butoxycarbonylamino-N-methylamino)-1-hexynyl]-6-methoxyquinazolin-4-yl}urea (0.1 g), trifluoroacetic acid (1 ml) and methylene chloride (1 ml) was stirred at ambient temperature for 1.5 hours. The mixture was evaporated and a solution of hydrogen chloride gas in ethyl acetate was added. Toluene was added and the mixture was evaporated. The residue was triturated under diethyl ether and the resultant solid was isolated. There was thus obtained the title compound as the hydrochloride salt (0.095 g); NMR Spectrum: (DMSOd6) 1.65 (m, 2H), 1.78 (m, 2H), 2.55 (m, 5H), 2.95 (m, 2H), 4.0 (s, 3H), 7.38 (t, 1H), 7.6 (d, 2H), 7.89 (s, 1H), 8.16 (s, 1H), 8.7 (m, 3H), 10.9 (br, 1H), 11.8 (s, 1H); Mass Spectrum: M+H+ 472 and 474.

後処理

  1. customThe mixture was evaporated
  2. additiona solution of hydrogen chloride gas in ethyl acetate was added
  3. additionToluene was added
  4. customthe mixture was evaporated
  5. customThe residue was triturated under diethyl ether
  6. customthe resultant solid was isolated

出典と根拠

ORDレコード
ord-292f1246fbbb4c0eae6c87d77ea770cb
出典データセット
uspto-grants-2004_10
特許番号
US06806274B1

反応ノート

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