Citric Acid → HCID 54767922, 화합물

HRID 472772노트

반응식

HRID 472772 반응식
[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

참가 물질

5

반응물 3

HCID 311Citric AcidHCID 8900Heptane2회HCID 46207586Ilorasertib

생성물 1

HCID 54767922HCID 54767922, 화합물

시약·촉매·용매 1

HCID 21881883Oxolane--water (1/1)용매2회

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-936710ba4eb84f27b3009a94c5a42370
출처 데이터셋
uspto-grants-2014_01
특허 번호
US08633217B2

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