Hydrochloric Acid → N-(3-{6-[amino(dicyclopropyl)methyl]pyridin-3-yl}-5-methylphenyl)-4-(trifluoromethyl)pyrimidin-2-amine

HRID 2207412노트

반응식

HRID 2207412 반응식
CO.Cl.[CH:4]1([C:7]([CH:39]2[CH2:41][CH2:40]2)([C:15]2[CH:20]=[CH:19][C:18]([C:21]3[CH:26]=[C:25]([NH:27][C:28]4[N:33]=[C:32]([C:34]([F:37])([F:36])[F:35])[CH:31]=[CH:30][N:29]=4)[CH:24]=[C:23]([CH3:38])[CH:22]=3)=[CH:17][N:16]=2)[NH:8][S@@](C(C)(C)C)=O)[CH2:6][CH2:5]1>O1CCOCC1.C([O-])(O)=O.[Na+]>[NH2:8][C:7]([CH:39]1[CH2:41][CH2:40]1)([CH:4]1[CH2:6][CH2:5]1)[C:15]1[N:16]=[CH:17][C:18]([C:21]2[CH:26]=[C:25]([NH:27][C:28]3[N:33]=[C:32]([C:34]([F:37])([F:36])[F:35])[CH:31]=[CH:30][N:29]=3)[CH:24]=[C:23]([CH3:38])[CH:22]=2)=[CH:19][CH:20]=1

참가 물질

6

반응물 3

HCID 313Hydrochloric Acid2회HCID 887MethanolHCID 131735914(R)-N-{dicyclopropyl[5-(3-methyl-5-{[4-(trifluoromethyl)pyrimidin-2-yl]amino}phenyl)pyridin-2-yl]methyl}-2-methylpropane-2-sulfinamide

생성물 1

HCID 118092744N-(3-{6-[amino(dicyclopropyl)methyl]pyridin-3-yl}-5-methylphenyl)-4-(trifluoromethyl)pyrimidin-2-amine

시약·촉매·용매 2

HCID 312751,4-Dioxane용매HCID 516892Sodium Bicarbonate용매

실험 절차

Methanol (5.00 mL) and HCl (4 M in dioxanes, 0.584 mL, 2.34 mmol) were added to (R)—N-{dicyclopropyl[5-(3-methyl-5-{[4-(trifluoromethyl)pyrimidin-2-yl]amino}phenyl)pyridin-2-yl]methyl}-2-methylpropane-2-sulfinamide (317.5 mg, 0.584 mmol) and the reaction mixture was stirred for 25 minutes at room temperature. An additional 150 uL of 4 M HCl in dioxane was added to the reaction mixture, stirred for 45 minutes, diluted with saturated aqueous NaHCO3 (20.0 mL) and extracted with ethyl acetate (30.0 mL). The organic layer was washed with brine, dried over sodium sulfate, filtered, and was concentrated under reduced pressure to yield N-(3-{6-[amino(dicyclopropyl)methyl]pyridin-3-yl}-5-methylphenyl)-4-(trifluoromethyl)pyrimidin-2-amine. MS APCI calc'd for C24H25F3N5 [M+H]+ 440. found 440.

후처리

  1. stirringstirred for 45 minutes
  2. extractionextracted with ethyl acetate (30.0 mL)
  3. washThe organic layer was washed with brine
  4. dry with materialdried over sodium sulfate
  5. filtrationfiltered
  6. concentrationwas concentrated under reduced pressure

출처 및 근거

ORD 기록
ord-1d92722aa77d41be861598d8b547870b
출처 데이터셋
uspto-grants-2016_06
특허 번호
US09376418B2

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