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3-Hydroxyazetidine hydrochloride → HCID 71280909, 화합물

HRID 246422
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HRID 246422 반응식
[C:1]([NH:5][C:6]([C:8]1[C:16]2[C:11](=[N:12][CH:13]=[C:14]([C:17]3[C:25]4[C:20](=[CH:21][CH:22]=[C:23]([O:26][CH:27]([F:29])[F:28])[CH:24]=4)[N:19]([CH2:30][CH2:31][CH:32]=O)[N:18]=3)[N:15]=2)[N:10]([CH2:34][O:35][CH2:36][CH2:37][Si:38]([CH3:41])([CH3:40])[CH3:39])[CH:9]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2].Cl.[NH:43]1[CH2:46][CH:45]([OH:47])[CH2:44]1.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>ClC(Cl)C.C([O-])(O)=O.[Na+]>[C:1]([NH:5][C:6]([C:8]1[C:16]2[C:11](=[N:12][CH:13]=[C:14]([C:17]3[C:25]4[C:20](=[CH:21][CH:22]=[C:23]([O:26][CH:27]([F:29])[F:28])[CH:24]=4)[N:19]([CH2:30][CH2:31][CH2:32][N:43]4[CH2:46][CH:45]([OH:47])[CH2:44]4)[N:18]=3)[N:15]=2)[N:10]([CH2:34][O:35][CH2:36][CH2:37][Si:38]([CH3:41])([CH3:40])[CH3:39])[CH:9]=1)=[O:7])([CH3:4])([CH3:3])[CH3:2]
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참가 물질

6

반응물 3

HCID 27592903-Hydroxyazetidine hydrochlorideHCID 5049666Sodium triacetoxyborohydrideHCID 86677979HCID 86677979, 화합물

생성물 1

HCID 71280909HCID 71280909, 화합물

시약·촉매·용매 2

HCID 63651,1-Dichloroethane용매HCID 516892Sodium Bicarbonate
용매

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온도
25 °C

실험 절차

To a solution of N-tert-butyl-2-(5-(difluoromethoxy)-1-(3-oxopropyl)-1H-indazol-3-yl)-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxamide (27 mg, 46.0 mmol) in dichloroethane (4.76 mL) was added azetidin-3-ol hydrochloride (6.55 mg, 59.8 μmol.30). The mixture was stirred at 25° C. for 15 min, then sodium triacetoxyborohydride (14.6 mg, 69.0 μmol0) was added and stirring was continued for 18 h. The reaction mixture was diluted with saturated NaHCO3 solution and extracted with dichloromethane (5×20 mL). The organic layer was dried (MgSO4) and concentrated in vacuo. The resultant residue was purified by chromatography (spherical silica 20-45 μm, 23 g, Versaflash Supelco) eluting with 0 to 5% over 20 min (MeOH containing 10% ammonium hydroxide)/dichloromethane to give traces of N-tert-butyl-2-(5-(difluoromethoxy)-1-(3-(3-hydroxyazetidin-1-yl)propyl)-1H-indazol-3-yl)-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxamide and obtained mainly N-tert-butyl-2-(5-(difluoromethoxy)-1-(3-hydroxypropyl)-1H-indazol-3-yl)-5-((2-(trimethylsilyl)ethoxy)methyl)-5H-pyrrolo[2,3-b]pyrazine-7-carboxamide (17 mg, 28.9 μmol, 62.7%) as an off-white solid. MS (M+H)+=589; 1H NMR (CDCl3) δ: 9.21 (s, 1H), 8.37 (s, 1H), 8.32 (d, J=2.3 Hz, 1H), 8.06 (s, 1H), 7.59 (d, J=9.1 Hz, 1H), 7.37 (dd, J=8.9, 2.1 Hz, 1H), 6.55 (t, J=74.4 Hz, 1H), 5.75 (s, 2H), 4.70 (t, J=6.6 Hz, 2H), 3.74 (t, J=5.7 Hz, 2H), 3.55-3.67 (m, 2H), 2.29 (quin, J=6.0 Hz, 2H), 1.64 (s, 9H), 0.91-1.05 (m, 2H), 0.00 (s, 9H).

후처리

  1. stirringstirring
  2. waitwas continued for 18 h
  3. extractionextracted with dichloromethane (5×20 mL)
  4. dry with materialThe organic layer was dried (MgSO4)
  5. concentrationconcentrated in vacuo
  6. customThe resultant residue was purified by chromatography (spherical silica 20-45 μm, 23 g, Versaflash Supelco)
  7. washeluting with 0 to 5% over 20 min (MeOH containing 10% ammonium hydroxide)/dichloromethane

출처 및 근거

ORD 기록
ord-b18f3507992d44aa835b8bddb7eeac2e
출처 데이터셋
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08658646B2

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