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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 471224
ノート
印刷プレビュー

反応式

HRID 471224 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 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

生成物 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

試薬・触媒・溶媒 1

HCID 887Methanol溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-078a1dce92934e30a83969148463c8ad
出典データセット
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08629271B2

反応ノート

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