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Hydrogen Peroxide → N-{1-[3,5-bis(trifluoromethyl)phenyl]ethyl}-N-({2-[(cyclopentylmethyl)(ethyl)amino]-5-(trifluoromethyl)phenyl}methyl)-5-[2-(methylsulfonyl)ethoxy]pyrimidin-2-amine

HRID 1442516
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HRID 1442516 반응식
[F:1][C:2]([F:48])([F:47])[C:3]1[CH:4]=[C:5]([CH:13]([N:15]([CH2:27][C:28]2[CH:33]=[C:32]([C:34]([F:37])([F:36])[F:35])[CH:31]=[CH:30][C:29]=2[N:38]([CH2:41][CH:42]2[CH2:46][CH2:45][CH2:44][CH2:43]2)[CH2:39][CH3:40])[C:16]2[N:21]=[CH:20][C:19]([O:22][CH2:23][CH2:24][S:25][CH3:26])=[CH:18][N:17]=2)[CH3:14])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.OO.[S:51]([O-:54])([O-])=[O:52].[Na+].[Na+].[C:57](#N)C>[Cl-].[Cl-].[Mo+2](=O)=O>[F:48][C:2]([F:1])([F:47])[C:3]1[CH:4]=[C:5]([CH:13]([N:15]([CH2:27][C:28]2[CH:33]=[C:32]([C:34]([F:35])([F:36])[F:37])[CH:31]=[CH:30][C:29]=2[N:38]([CH2:41][CH:42]2[CH2:43][CH2:44][CH2:45][CH2:46]2)[CH2:39][CH3:40])[C:16]2[N:17]=[CH:18][C:19]([O:22][CH2:23][CH2:24][S:25]([CH3:26])=[O:52])=[CH:20][N:21]=2)[CH3:14])[CH:6]=[C:7]([C:9]([F:12])([F:11])[F:10])[CH:8]=1.[F:48][C:2]([F:1])([F:47])[C:3]1[CH:4]=[C:5]([CH:13]([N:15]([CH2:27][C:28]2[CH:33]=[C:32]([C:34]([F:35])([F:36])[F:37])[CH:31]=[CH:30][C:29]=2[N:38]([CH2:41][CH:42]2[CH2:43][CH2:44][CH2:45][CH2:46]2)[CH2:39][CH3:40])[C:16]2[N:17]=[CH:18][C:19]([O:22][CH2:23][CH2:24][S:51]([CH3:57])(=[O:54])=[O:52])=[CH:20][N:21]=2)[CH3:14])[CH:6]=[C:7]([C:9]([F:10])([F:12])[F:11])[CH:8]=1
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반응물 4

HCID 784Hydrogen PeroxideHCID 6342AcetonitrileHCID 24437Sodium SulfiteHCID 25056258N-{1-[3,5-bis(trifluoromethyl)phenyl]ethyl}-N-({2-[(cyclopentylmethyl)(ethyl)amino]-5-(trifluoromethyl)phenyl}methyl)-5-[2-(methylthio)ethoxy]pyrimidin-2-amine

생성물 2

HCID 25022380
N-{1-[3,5-bis(trifluoromethyl)phenyl]ethyl}-N-({2-[(cyclopentylmethyl)(ethyl)amino]-5-(trifluoromethyl)phenyl}methyl)-5-[2-(methylsulfonyl)ethoxy]pyrimidin-2-amine
수율 81%
HCID 25056259N-{1-[3,5-bis(trifluoromethyl)phenyl]ethyl}-N-({2-[(cyclopentylmethyl)(ethyl)amino]-5-(trifluoromethyl)phenyl}methyl)-5-[2-(methylsulfinyl)ethoxy]pyrimidin-2-amine수율 9%

시약·촉매·용매 1

HCID 86628431Dioxomolybdenum(2+) dichloride촉매

실험 절차

To a solution of N-{1-[3,5-bis(trifluoromethyl)phenyl]ethyl}-N-({2-[(cyclopentylmethyl)(ethyl)amino]-5-(trifluoromethyl)phenyl}methyl)-5-[2-(methylthio)ethoxy]pyrimidin-2-amine (348 mg, 0.49 mmol) obtained in Example 1 in acetonitrile (7 mL) was added molybdenum dioxide dichloride (14.6 mg, 0.073 mmol) and 30% aqueous hydrogen peroxide (220 mg, 1.94 mmol), and the mixture was stirred at room temperature for 23 hours. The reaction mixture was added with saturated aqueous sodium sulfite, and extracted with chloroform. Then, the organic layer was washed with saturated brine, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The resulting residue was purified by preparative silica gel thin layer chromatography (hexane:acetone=2:1) to obtain N-{1-[3,5-bis(trifluoromethyl)phenyl]ethyl}-N-({2-[(cyclopentylmethyl)(ethyl)amino]-5-(trifluoromethyl)phenyl}methyl)-5-[2-(methylsulfinyl)ethoxy]pyrimidin-2-amine (compound of Example 2, 32.8 mg, 9%) as yellow oil, and N-{1-[3,5-bis(trifluoromethyl)phenyl]ethyl}-N-({2-[(cyclopentylmethyl)(ethyl)amino]-5-(trifluoromethyl)phenyl}methyl)-5-[2-(methylsulfonyl)ethoxy]pyrimidin-2-amine (compound of Example 3, 295 mg, 81%) as a pale yellow oil.

후처리

  1. extractionextracted with chloroform
  2. washThen, the organic layer was washed with saturated brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. concentrationconcentrated under reduced pressure
  5. customThe resulting residue was purified by preparative silica gel thin layer chromatography (hexane:acetone=2:1)

출처 및 근거

ORD 기록
ord-80bcb99dacbf4454b668a4c00750a81d
출처 데이터셋
uspto-grants-2010_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07659271B2

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