Citric Acid → HCID 54767922、化合物

HRID 472772ノート

反応式

HRID 472772 の反応式
[NH2:1][C:2]1[C:7]2[C:8]([C:11]3[CH:16]=[CH:15][C:14]([NH:17][C:18]([NH:20][C:21]4[CH:26]=[CH:25][CH:24]=[C:23]([F:27])[CH:22]=4)=[O:19])=[CH:13][CH:12]=3)=[CH:9][S:10][C:6]=2[C:5]([C:28]2[CH:29]=[N:30][N:31]([CH2:33][CH2:34][OH:35])[CH:32]=2)=[CH:4][N:3]=1.[C:36]([OH:48])(=[O:47])[CH2:37][C:38]([CH2:43][C:44]([OH:46])=[O:45])([C:40]([OH:42])=[O:41])[OH:39].CCCCCCC>C1COCC1.O>[C:36]([OH:48])(=[O:47])[CH2:37][C:38]([CH2:43][C:44]([OH:46])=[O:45])([C:40]([OH:42])=[O:41])[OH:39].[NH2:1][C:2]1[C:7]2[C:8]([C:11]3[CH:12]=[CH:13][C:14]([NH:17][C:18]([NH:20][C:21]4[CH:26]=[CH:25][CH:24]=[C:23]([F:27])[CH:22]=4)=[O:19])=[CH:15][CH:16]=3)=[CH:9][S:10][C:6]=2[C:5]([C:28]2[CH:29]=[N:30][N:31]([CH2:33][CH2:34][OH:35])[CH:32]=2)=[CH:4][N:3]=1

参加物

5

反応物 3

HCID 311Citric AcidHCID 8900Heptane2 回HCID 46207586Ilorasertib

生成物 1

HCID 54767922HCID 54767922、化合物

試薬・触媒・溶媒 1

HCID 21881883Oxolane--water (1/1)溶媒2 回

実験手順

N-(4-{4-amino-7-[1-(2-hydroxyethyl)-1H-pyrazol-4-yl]thieno[3,2-c]pyridin-3-yl}phenyl)-N′-(3-fluorophenyl)urea free base solid (102.65 mg) was dissolved in 5 mL of THF/water mixture (80/20 v/v) at 70° C. Citric acid (21.94 mg) was added to the solution followed by the slow addition of heptane (7.5 mL). The appearance of a small amount of precipitant formed in the heptane layer was noted. The precipitant dissolved as it fell into the THF/water layer. The solution was cooled to ambient temperatures. Crystalline solids formed after several days at ambient temperatures. Solid was collected by vacuum filtration.

後処理

  1. dissolutionThe precipitant dissolved as it
  2. temperatureThe solution was cooled to ambient temperatures
  3. customCrystalline solids formed after several days at ambient temperatures
  4. filtrationSolid was collected by vacuum filtration

出典と根拠

ORDレコード
ord-936710ba4eb84f27b3009a94c5a42370
出典データセット
uspto-grants-2014_01
特許番号
US08633217B2

反応ノート

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