3-(Dimethylamino)-2,2-dimethyl-1-propanol → HCID 22594117、化合物

HRID 1760981

反応式

HRID 1760981 の反応式
Cl[C:2]1[N:7]=[C:6]([NH:8][C:9]2[CH:14]=[C:13]([NH:15][C:16]([C:18]3[C:23]4[O:24][C:25]5[CH:30]=[CH:29][CH:28]=[CH:27][C:26]=5[C:22]=4[CH:21]=[CH:20][CH:19]=3)=[O:17])[CH:12]=[CH:11][C:10]=2[CH3:31])[CH:5]=[CH:4][N:3]=1.[CH3:32][N:33]([CH3:40])[CH2:34][C:35]([CH3:39])([CH3:38])[CH2:36][OH:37]>>[CH:21]1[C:22]2[C:26]3[CH:27]=[CH:28][CH:29]=[CH:30][C:25]=3[O:24][C:23]=2[C:18]([C:16]([NH:15][C:13]2[CH:12]=[CH:11][C:10]([CH3:31])=[C:9]([CH:14]=2)[NH:8][C:6]2[CH:5]=[CH:4][N:3]=[C:2]([O:37][CH2:36][C:35]([CH3:39])([CH3:38])[CH2:34][N:33]([CH3:40])[CH3:32])[N:7]=2)=[O:17])=[CH:19][CH:20]=1

参加物

3

反応物 2

HCID 879193-(Dimethylamino)-2,2-dimethyl-1-propanolHCID 22594095HCID 22594095、化合物

生成物 1

HCID 22594117HCID 22594117、化合物

実験手順

Using an analogous procedure to that described in Example 8, 2-chloro-4-[5-(4-dibenzofuranylcarbonylamino)-2-methylanilino]pyrimidine was reacted with 3-dimethylamino-2,2-dimethylpropanol. The reaction mixture was evaporated and the residue was purified by column chromatography on silica using increasingly polar mixtures of methylene chloride and methanol as eluent followed by increasingly polar mixtures of methylene chloride and methanol containing 1% aqueous ammonium hydroxide solution. There was thus obtained the title compound; NMR Spectrum: (DMSOd6) 0.85 (s, 6H), 2.14 (s, 6H), 2.18 (s, 2H), 3.94 (s, 2H), 6.22 (d, 1H), 7.23 (d, 1H), 7.4-7.58 (m, 4H), 7.78 (d, 1H), 7.84 (d, 1H), 7.96 (m, 2H), 8.2 (d, 1H), 8.31 (d, 1H); Mass Spectrum: M+H+ 524.

後処理

  1. customThe reaction mixture was evaporated
  2. customthe residue was purified by column chromatography on silica using
  3. temperatureincreasingly polar mixtures of methylene chloride and methanol as eluent
  4. temperatureby increasingly polar mixtures of methylene chloride and methanol containing 1% aqueous ammonium hydroxide solution

出典と根拠

ORDレコード
ord-3fae238040344cc0998edd6d90fabd81
出典データセット
uspto-grants-2005_01
特許番号
US06846827B1

関連ノート

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