Water → HCID 67200711, 화합물

HRID 509975노트

반응식

HRID 509975 반응식
C1(S([N:10]2[C:14]3=[N:15][CH:16]=[C:17]([O:19][CH3:20])[CH:18]=[C:13]3[C:12]([CH2:21][C:22]3[CH:23]=[N:24][C:25]([NH:28][CH2:29][C:30]4[C:31]([O:37][CH3:38])=[N:32][CH:33]=[C:34]([F:36])[CH:35]=4)=[N:26][CH:27]=3)=[CH:11]2)(=O)=O)C=CC=CC=1.O.O.O.[F-].C([N+](CCCC)(CCCC)CCCC)CCC.O>O1CCCC1>[F:36][C:34]1[CH:35]=[C:30]([CH2:29][NH:28][C:25]2[N:26]=[CH:27][C:22]([CH2:21][C:12]3[C:13]4[C:14](=[N:15][CH:16]=[C:17]([O:19][CH3:20])[CH:18]=4)[NH:10][CH:11]=3)=[CH:23][N:24]=2)[C:31]([O:37][CH3:38])=[N:32][CH:33]=1

참가 물질

5

반응물 3

HCID 962WaterHCID 11726816Tetrabutylammonium Fluoride TrihydrateHCID 67200202HCID 67200202, 화합물

생성물 1

HCID 67200711HCID 67200711, 화합물

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

To [5-(1-benzenesulfonyl-5-methoxy-1H-pyrrolo[2,3-b]pyridin-3-ylmethyl)-pyrimidin-2-yl]-(5-fluoro-2-methoxy-pyridin-3-ylmethyl)-amine (125, 1 equivalent) in 15.0 mL of tetrahydrofuran, tetrabutylammonium fluoride trihydrate (2 equivalent) is added. The reaction is stirred at room temperature overnight, then poured into water and extracted with ethyl acetate. The organic layer is dried over sodium sulfate, filtered and the filtrate concentrated under vacuum. The resulting material is purified by silica gel column chromatography eluting with 20-100% ethyl acetate in hexane. Appropriate fractions are combined and concentrated under vacuum to provide the desired compound as a yellow solid.

후처리

  1. extractionextracted with ethyl acetate
  2. dry with materialThe organic layer is dried over sodium sulfate
  3. filtrationfiltered
  4. concentrationthe filtrate concentrated under vacuum
  5. customThe resulting material is purified by silica gel column chromatography
  6. washeluting with 20-100% ethyl acetate in hexane
  7. concentrationconcentrated under vacuum

출처 및 근거

ORD 기록
ord-970d0ecfb0fa4a71ba0a2e877ba066d7
출처 데이터셋
uspto-grants-2015_08
특허 번호
US09096593B2

반응 노트

불러오는 중…