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

HRID 393246노트

반응식

HRID 393246 반응식
[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]

참가 물질

4

반응물 2

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

생성물 1

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

시약·촉매·용매 1

HCID 6344Dichloromethane용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-292f1246fbbb4c0eae6c87d77ea770cb
출처 데이터셋
uspto-grants-2004_10
특허 번호
US06806274B1

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