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Cesium carbonate → HCID 58386633、化合物

HRID 74678
ノート
印刷プレビュー

反応式

HRID 74678 の反応式
C1C=CC(P(C2C(C3C(P(C4C=CC=CC=4)C4C=CC=CC=4)=CC=C4C=3C=CC=C4)=C3C(C=CC=C3)=CC=2)C2C=CC=CC=2)=CC=1.[CH3:47][O:48][C:49]1[CH:50]=[CH:51][C:52]2[NH:58][C:57](=[O:59])[N:56]([CH:60]3[CH2:65][CH2:64][NH:63][CH2:62][CH2:61]3)[CH2:55][CH2:54][C:53]=2[CH:66]=1.Br[C:68]1[CH:69]=[N+:70]([O-:86])[CH:71]=[C:72]([C:74]([N:76]2[C:84]3[C:79](=[CH:80][C:81]([F:85])=[CH:82][CH:83]=3)[CH2:78][CH2:77]2)=[O:75])[CH:73]=1.C(=O)([O-])[O-].[Cs+].[Cs+]>O1CCOCC1.C([O-])(=O)C.[Pd+2].C([O-])(=O)C>[F:85][C:81]1[CH:80]=[C:79]2[C:84](=[CH:83][CH:82]=1)[N:76]([C:74]([C:72]1[CH:71]=[N+:70]([O-:86])[CH:69]=[C:68]([N:63]3[CH2:64][CH2:65][CH:60]([N:56]4[CH2:55][CH2:54][C:53]5[CH:66]=[C:49]([O:48][CH3:47])[CH:50]=[CH:51][C:52]=5[NH:58][C:57]4=[O:59])[CH2:61][CH2:62]3)[CH:73]=1)=[O:75])[CH2:77][CH2:78]2
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 10796Cesium carbonateHCID 634876Binap, (A+-)-HCID 183568527-methoxy-3-(piperidin-4-yl)-4,5-dihydro-1H-benzo[d][1,3]diazepin-2(3H)-oneHCID 673382653-Bromo-5-(5-fluoroindoline-1-carbonyl)-pyridine-1-oxide

生成物 1

HCID 58386633HCID 58386633、化合物

試薬・触媒・溶媒 2

HCID 167845
palladium(II) acetate
触媒
HCID 312751,4-Dioxane溶媒

反応条件

温度
120 °C

実験手順

Under an argon atmosphere 5.0 mg (0.02 mmol) palladium(II)acetate and 14 mg (20 μmol) BINAP were added to 69 mg (0.25 mmol) 7-methoxy-3-piperidin-4-yl-1,3,4,5-tetrahydro-1,3-benzodiazepin-2-one, 84 mg (0.25 mmol) 3-bromo-5-(5-fluoroindoline-1-carbonyl)-pyridine-1-oxide and 0.12 g (0.38 mmol) caesium carbonate in 4.0 mL dioxane and the mixture was stirred overnight at 120° C. The reaction mixture was then evaporated down and the residue was dissolved in DMF/MeOH and purified by preparative HPLC-MS. The product-containing fractions were combined, the organic solvent was evaporated down and the residue was made alkaline with a 1N aqueous sodium hydroxide solution. The precipitate formed was suction filtered, washed with water and dried under HV.

後処理

  1. customThe reaction mixture was then evaporated down
  2. dissolutionthe residue was dissolved in DMF/MeOH
  3. custompurified by preparative HPLC-MS
  4. customthe organic solvent was evaporated down
  5. customThe precipitate formed
  6. filtrationfiltered
  7. washwashed with water
  8. customdried under HV

出典と根拠

ORDレコード
ord-1b72a5099787497b801e1bf8665068c0
出典データセット
uspto-grants-2014_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08829006B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート