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llms.txt · MCP 가이드개인정보처리방침 · 이용약관 · 지원v1.8.0
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Acetic Acid → (R)-5-(1-(tert-Butyldimethylsilyloxy)-2-(3-((4-(2-methylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)methyl)benzylamino)ethyl)-8-hydroxyquinolin-2(1H)-one

HRID 1689455
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HRID 1689455 반응식
[CH3:1][C:2]1[S:3][CH:4]=[C:5]([C:7]([N:9]2[CH2:14][C:13]3([CH2:19][CH2:18][N:17]([CH2:20][C:21]4[CH:22]=[C:23]([CH:26]=[CH:27][CH:28]=4)[CH:24]=O)[CH2:16][CH2:15]3)[O:12][CH2:11][CH2:10]2)=[O:8])[N:6]=1.[NH2:29][CH2:30][C@@H:31]([C:40]1[CH:49]=[CH:48][C:47]([OH:50])=[C:46]2[C:41]=1[CH:42]=[CH:43][C:44](=[O:51])[NH:45]2)[O:32][Si:33]([C:36]([CH3:39])([CH3:38])[CH3:37])([CH3:35])[CH3:34].C(O)(=O)C.C(O[BH-](OC(=O)C)OC(=O)C)(=O)C.[Na+]>CO>[Si:33]([O:32][C@H:31]([C:40]1[CH:49]=[CH:48][C:47]([OH:50])=[C:46]2[C:41]=1[CH:42]=[CH:43][C:44](=[O:51])[NH:45]2)[CH2:30][NH:29][CH2:24][C:23]1[CH:26]=[CH:27][CH:28]=[C:21]([CH2:20][N:17]2[CH2:16][CH2:15][C:13]3([O:12][CH2:11][CH2:10][N:9]([C:7]([C:5]4[N:6]=[C:2]([CH3:1])[S:3][CH:4]=4)=[O:8])[CH2:14]3)[CH2:19][CH2:18]2)[CH:22]=1)([C:36]([CH3:39])([CH3:38])[CH3:37])([CH3:35])[CH3:34]
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참가 물질

6

반응물 4

HCID 176Acetic AcidHCID 5049666Sodium triacetoxyborohydrideHCID 579889313-((4-(2-Methylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)methyl)benzaldehydeHCID 59023604(R)-5-(2-Amino-1-((tert-butyldimethylsilyl)oxy)ethyl)-8-hydroxyquinolin-2(1H)-one

생성물 1

HCID 57989240
(R)-5-(1-(tert-Butyldimethylsilyloxy)-2-(3-((4-(2-methylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)methyl)benzylamino)ethyl)-8-hydroxyquinolin-2(1H)-one

시약·촉매·용매 1

HCID 887Methanol용매

실험 절차

A solution of 3-((4-(2-methylthiazole-4-carbonyl)-1-oxa-4,9-diazaspiro[5.5]undecan-9-yl)methyl)benzaldehyde (example 96, step a) (0.303 g), (R)-5-(2-amino-1-(tert-butyldimethylsilyloxy)ethyl)-8-hydroxyquinolin-2(1H)-one (WO2004106333) (0.330 g) and acetic acid (0.043 mL) in methanol (5 mL) was stirred at room temperature for 30 minutes, then cooled in an ice-water bath under nitrogen and treated with sodium triacetoxyborohydride (0.243 g) in one portion. The mixture was stirred in ice-water for 2 hours, then concentrated in vacuo. The residue was partitioned between ethyl acetate and saturated sodium bicarbonate solution, the phases were separated, and the aqueous phase was extracted twice more with ethyl acetate. Any insoluble gummy residues were dissolved in methanol. The combined ethyl acetate phases were washed with brine, dried over magnesium sulphate and combined with the methanol solution. The whole was purified by flash chromatography on silica eluted with 1:7:92 triethylamine:methanol:dichloromethane to afford the slightly impure subtitled product as a yellow foam. Yield 0.324 g.

후처리

  1. temperaturecooled in an ice-water bath under nitrogen
  2. concentrationconcentrated in vacuo
  3. customThe residue was partitioned between ethyl acetate and saturated sodium bicarbonate solution
  4. customthe phases were separated
  5. extractionthe aqueous phase was extracted twice more with ethyl acetate
  6. dissolutionAny insoluble gummy residues were dissolved in methanol
  7. washThe combined ethyl acetate phases were washed with brine
  8. dry with materialdried over magnesium sulphate
  9. customThe whole was purified by flash chromatography on silica
  10. washeluted with 1:7:92 triethylamine

출처 및 근거

ORD 기록
ord-a894ddf63b224649845a7d54a9da253f
출처 데이터셋
uspto-grants-2012_04
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US08148373B2

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