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Binap, (A+-)- → 2-(4-tert-butoxycarbonylbenzyl)-6-[4-(5-methyl-3-phenylisoxazol-4-yl)pyrimidin-2-ylamino]-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic Acid Methyl Ester

HRID 750260
ノート
印刷プレビュー

反応式

HRID 750260 の反応式
C1(P(C2C=CC=CC=2)C2C=CC3C(=CC=CC=3)C=2C2C3C(=CC=CC=3)C=CC=2P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.[CH3:47][O:48][C:49]([C:51]1[N:52]([CH2:69][C:70]2[CH:75]=[CH:74][C:73]([C:76]([O:78][C:79]([CH3:82])([CH3:81])[CH3:80])=[O:77])=[CH:72][CH:71]=2)[C:53](=[O:68])[C:54]2[C:59]([C:60]=1[C:61]1[CH:66]=[CH:65][CH:64]=[CH:63][CH:62]=1)=[CH:58][C:57](Br)=[CH:56][CH:55]=2)=[O:50].[CH3:83][C:84]1[O:88][N:87]=[C:86]([C:89]2[CH:94]=[CH:93][CH:92]=[CH:91][CH:90]=2)[C:85]=1[C:95]1[CH:100]=[CH:99][N:98]=[C:97]([NH2:101])[N:96]=1.CC(C)([O-])C.[Na+]>C([O-])(=O)C.[Pd+2].C([O-])(=O)C.O.C1(C)C=CC=CC=1>[CH3:47][O:48][C:49]([C:51]1[N:52]([CH2:69][C:70]2[CH:75]=[CH:74][C:73]([C:76]([O:78][C:79]([CH3:82])([CH3:81])[CH3:80])=[O:77])=[CH:72][CH:71]=2)[C:53](=[O:68])[C:54]2[C:59]([C:60]=1[C:61]1[CH:66]=[CH:65][CH:64]=[CH:63][CH:62]=1)=[CH:58][C:57]([NH:101][C:97]1[N:96]=[C:95]([C:85]3[C:86]([C:89]4[CH:90]=[CH:91][CH:92]=[CH:93][CH:94]=4)=[N:87][O:88][C:84]=3[CH3:83])[CH:100]=[CH:99][N:98]=1)=[CH:56][CH:55]=2)=[O:50]
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 634876Binap, (A+-)-HCID 27457214-(5-Methyl-3-phenylisoxazol-4-yl)pyrimidin-2-amineHCID 23676156Sodium t-butoxideHCID 691566226-bromo-2-(4-tert-butoxycarbonylbenzyl)-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic Acid Methyl Ester

生成物 1

HCID 69156270
2-(4-tert-butoxycarbonylbenzyl)-6-[4-(5-methyl-3-phenylisoxazol-4-yl)pyrimidin-2-ylamino]-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic Acid Methyl Ester
収率 61%

試薬・触媒・溶媒 3

HCID 167845palladium(II) acetate触媒HCID 962Water溶媒HCID 1140Toluene溶媒

実験手順

To toluene (6 ml) were added palladium(II) acetate (4.1 mg) and rac-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (34 mg) at room temperature and the mixture was stirred for 5 min. under a nitrogen stream. To the reaction mixture were added 6-bromo-2-(4-tert-butoxycarbonylbenzyl)-1-oxo-4-phenyl-1,2-dihydroisoquinoline-3-carboxylic acid methyl ester (300 mg) and 4-(5-methyl-3-phenylisoxazol-4-yl)pyrimidin-2-ylamine (200 mg) at room temperature and the mixture was stirred for 10 min. under a nitrogen stream. Further, sodium tert-butoxide (70 mg) was added to the reaction mixture at room temperature, and the mixture was heated under reflux under a nitrogen atmosphere for 12 hrs. Water was added to the reaction mixture and the mixture was extracted with ethyl acetate. The organic layer was washed with water, saturated brine and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure and the obtained residue was purified by silica gel column chromatography (hexane-hexane:ethyl acetate=1:1), followed by recrystallization (ethyl acetate-hexane) to give the title compound (240 mg).

後処理

  1. stirringthe mixture was stirred for 10 min. under a nitrogen stream
  2. temperaturethe mixture was heated
  3. temperatureunder reflux under a nitrogen atmosphere for 12 hrs
  4. extractionthe mixture was extracted with ethyl acetate
  5. washThe organic layer was washed with water, saturated brine
  6. dry with materialdried over anhydrous sodium sulfate
  7. customThe solvent was evaporated under reduced pressure
  8. customthe obtained residue was purified by silica gel column chromatography (hexane-hexane:ethyl acetate=1:1)
  9. customfollowed by recrystallization (ethyl acetate-hexane)

出典と根拠

ORDレコード
ord-da29f78e6f8d4047bcaef94a8fe44945
出典データセット
uspto-grants-2008_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07402595B2

反応ノート

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