Hydrochloric Acid → 5-Amino-6-chloro-4-[5-(3-fluoro-5-morpholinobenzamido) 2-methylanilino]pyrimidine

HRID 1760963

反応式

HRID 1760963 の反応式
Cl.[NH2:2][C:3]1[C:4]([Cl:10])=[N:5][CH:6]=[N:7][C:8]=1Cl.[NH2:11][C:12]1[CH:13]=[C:14]([NH:19][C:20](=[O:34])[C:21]2[CH:26]=[C:25]([N:27]3[CH2:32][CH2:31][O:30][CH2:29][CH2:28]3)[CH:24]=[C:23]([F:33])[CH:22]=2)[CH:15]=[CH:16][C:17]=1[CH3:18].C(NC(C)C)(C)C.CCCC(C)C>C(OCC)C.O.C(O)CCC>[NH2:2][C:3]1[C:8]([NH:11][C:12]2[CH:13]=[C:14]([NH:19][C:20](=[O:34])[C:21]3[CH:26]=[C:25]([N:27]4[CH2:28][CH2:29][O:30][CH2:31][CH2:32]4)[CH:24]=[C:23]([F:33])[CH:22]=3)[CH:15]=[CH:16][C:17]=2[CH3:18])=[N:7][CH:6]=[N:5][C:4]=1[Cl:10]

参加物

9

反応物 5

HCID 313Hydrochloric AcidHCID 78922-MethylpentaneHCID 7912DiisopropylamineHCID 794345-Amino-4,6-dichloropyrimidineHCID 11450304N-(3-amino-4-methylphenyl)-3-fluoro-5-morpholinobenzamide

生成物 1

HCID 867595915-Amino-6-chloro-4-[5-(3-fluoro-5-morpholinobenzamido) 2-methylanilino]pyrimidine収率 52.3%

試薬・触媒・溶媒 3

HCID 2631-Butanol溶媒HCID 962Water溶媒HCID 3283Diethyl Ether溶媒

実験手順

Ethereal hydrogen chloride solution (1M, 1.5 ml) was added to a mixture of 5-amino-4,6-dichloropyrimidine (0.512 g), N-(3-amino-4-methylphenyl)-3-fluoro-5-morpholinobenzamide (0.514 g) and n-butanol (10 ml) and the resultant mixture was stirred and heated to reflux for 24 hours. Di-isopropylamine (1 ml) was added and the mixture was allowed to cool to ambient temperature. Water and a mixture of diethyl ether and isohexane were added and the precipitated solid was collected and dried. There was thus obtained the title compound (0.373 g); NMR Spectrum: 2.12 (s, 3H), 3.22 (m, 4H), 3.74 (m, 4H), 5.28 (s, 2H), 6.87 (d, 1H), 7.11 (d, 1H), 7.22 (d. 1H), 7.27 (s, 1H), 7.52 (d, 1H), 7.69 (s, 1H), 7.73 (s, 1H), 8.03 (s, 1H), 10.15 (s, 1H); Mass Spectrum: M−H − 455 & 457.

後処理

  1. temperatureheated
  2. temperatureto reflux for 24 hours
  3. additionwere added
  4. customthe precipitated solid was collected
  5. customdried

出典と根拠

ORDレコード
ord-ad35486282904577b4a5b99697228caf
出典データセット
uspto-grants-2005_01
特許番号
US06846827B1

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