Hydrochloric Acid → N4-(3-Fluoro-4-{[3-(2-methoxyethyl)-1H-pyrrolo[2,3-b]pyridin-4-yl]oxy}phenyl)-6-(trifluoromethyl)pyrimidine-2,4-diamine

HRID 2192191노트

반응식

HRID 2192191 반응식
[F:1][C:2]1[CH:3]=[C:4]([CH:6]=[CH:7][C:8]=1[O:9][C:10]1[CH:15]=[CH:14][N:13]=[C:12]2[NH:16][CH:17]=[C:18]([CH2:19][CH2:20][O:21][CH3:22])[C:11]=12)[NH2:5].Cl[C:24]1[CH:29]=[C:28]([C:30]([F:33])([F:32])[F:31])[N:27]=[C:26]([NH2:34])[N:25]=1.Cl.N1C=CC=CC=1N.[OH-].[Na+]>O>[F:1][C:2]1[CH:3]=[C:4]([NH:5][C:24]2[CH:29]=[C:28]([C:30]([F:33])([F:31])[F:32])[N:27]=[C:26]([NH2:34])[N:25]=2)[CH:6]=[CH:7][C:8]=1[O:9][C:10]1[CH:15]=[CH:14][N:13]=[C:12]2[NH:16][CH:17]=[C:18]([CH2:19][CH2:20][O:21][CH3:22])[C:11]=12

참가 물질

7

반응물 5

HCID 313Hydrochloric AcidHCID 104392-AminopyridineHCID 14798Sodium HydroxideHCID 130869074-Chloro-6-(trifluoromethyl)pyrimidin-2-amineHCID 597410123-Fluoro-4-{[3-(2-methoxyethyl)-1H-pyrrolo[2,3-b]pyridin-4-yl]oxy}aniline

생성물 1

HCID 11547139N4-(3-Fluoro-4-{[3-(2-methoxyethyl)-1H-pyrrolo[2,3-b]pyridin-4-yl]oxy}phenyl)-6-(trifluoromethyl)pyrimidine-2,4-diamine

시약·촉매·용매 1

HCID 962Water용매

실험 절차

53 mg (0.18 mmol) of 3-fluoro-4-{[3-(2-methoxyethyl)-1H-pyrrolo[2,3-b]pyridin-4-yl]oxy}aniline and 42 mg (0.21 mmol) of 4-chloro-6-(trifluoromethyl)pyrimidine-2-amine are suspended in 4 ml of water. 0.23 ml (0.23 mmol) of 1N hydrochloric acid is added, and the mixture is heated at reflux overnight. Another 22 mg (0.11 mmol) of 4-chloro-6-trifluoromethyl)pyridine-2-amine are then added, and the mixture is again heated overnight. By addition of 1N aqueous sodium hydroxide solution, the pH is adjusted to 10, resulting in the precipitation of crystals. The crystals are filtered off with suction and washed with water. The product is purified by preparative HPLC.

후처리

  1. temperaturethe mixture is heated
  2. temperatureat reflux overnight
  3. customresulting in the precipitation of crystals
  4. filtrationThe crystals are filtered off with suction
  5. washwashed with water
  6. customThe product is purified by preparative HPLC

출처 및 근거

ORD 기록
ord-c0197804f99943078c389157244e86e4
출처 데이터셋
uspto-grants-2012_12
특허 번호
US08329716B2

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