Trifluoroacetic acid → HCID 178486747、化合物

HRID 228957

反応式

HRID 228957 の反応式
FC(F)(F)C(O)=O.[CH3:8][O:9][C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][C:19]=1[O:20][CH2:21][CH2:22][NH:23][C:24]([NH:33]C(OC(C)(C)C)=O)=[N:25]C(OC(C)(C)C)=O)[N:16]=[CH:15][CH:14]=[C:13]2[O:41][C:42]1[C:43]([CH3:52])=[N:44][C:45]2[C:50]([CH:51]=1)=[CH:49][CH:48]=[CH:47][CH:46]=2.[OH-].[Na+]>>[CH3:8][O:9][C:10]1[CH:11]=[C:12]2[C:17](=[CH:18][C:19]=1[O:20][CH2:21][CH2:22][NH:23][C:24]([NH2:33])=[NH:25])[N:16]=[CH:15][CH:14]=[C:13]2[O:41][C:42]1[C:43]([CH3:52])=[N:44][C:45]2[C:50]([CH:51]=1)=[CH:49][CH:48]=[CH:47][CH:46]=2

参加物

4

反応物 3

HCID 6422Trifluoroacetic acidHCID 14798Sodium HydroxideHCID 178486746HCID 178486746、化合物

生成物 1

HCID 178486747HCID 178486747、化合物収率 100%

反応条件

温度
0 °C

実験手順

Trifluoroacetic acid (1 ml) was added to N-{2-[6-methoxy-4-(2-methyl-quinolin-3-yloxy)-quinolin-7-yloxy]-ethyl}-N′,N″-diboc-guanidine (222 mg) at 0° C., and the mixture was then stirred at 0° C. for 2 hr. The reaction solution was made alkaline by the addition of a 1 N aqueous sodium hydroxide solution and was extracted with n-butanol. The n-butanol layer was washed with water and was then dried over anhydrous magnesium sulfate. The solvent was removed by distillation under the reduced pressure, and the residue was purified by thin layer chromatography using chloroform-methanol to give the title compound (150 mg, yield 100%).

後処理

  1. extractionwas extracted with n-butanol
  2. washThe n-butanol layer was washed with water
  3. dry with materialwas then dried over anhydrous magnesium sulfate
  4. customThe solvent was removed by distillation under the reduced pressure
  5. customthe residue was purified by thin layer chromatography

出典と根拠

ORDレコード
ord-1473569bef484c709de4853e270842aa
出典データセット
uspto-grants-2009_07
特許番号
US07560558B2

関連ノート

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