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Dichloromethane → 1-(Phenylacetyl)-5-(4-pyridinyl)indoline

HRID 1510253
ノート
印刷プレビュー

反応式

HRID 1510253 の反応式
Br[C:2]1[CH:3]=[C:4]2[C:8](=[CH:9][CH:10]=1)[N:7]([C:11](=[O:19])[CH2:12][C:13]1[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1)[CH2:6][CH2:5]2.CC1(C)C(C)(C)OB([C:28]2[CH:33]=[CH:32][N:31]=[CH:30][CH:29]=2)O1.ClCCl.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>COCCOC.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.C1C=CC(P(C2C=CC=CC=2)[C-]2C=CC=C2)=CC=1.Cl[Pd]Cl.[Fe+2]>[C:13]1([CH2:12][C:11]([N:7]2[C:8]3[C:4](=[CH:3][C:2]([C:28]4[CH:33]=[CH:32][N:31]=[CH:30][CH:29]=4)=[CH:10][CH:9]=3)[CH2:5][CH2:6]2)=[O:19])[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=1
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 6344DichloromethaneHCID 62657Potassium Phosphate, TribasicHCID 27346484-(4,4,5,5-Tetramethyl-1,3,2-dioxaborolan-2-yl)pyridineHCID 668241055-bromo-1-(phenylacetyl)-2,3-dihydro-1H-indole

生成物 1

HCID 576639941-(Phenylacetyl)-5-(4-pyridinyl)indoline収率 50.5%

試薬・触媒・溶媒 2

HCID 44119782
Bis(cyclopenta-1,4-dien-1-yl(diphenyl)phosphane);dichloropalladium;iron(2+)
触媒
HCID 80711,2-Dimethoxyethane溶媒

反応条件

温度
100 °C

実験手順

To a solution of 5-bromo-1-(phenylacetyl)indoline (15.98 g) and 4-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)pyridine (12.4 g) in 1,2-dimethoxyethane (500 mL) were added [1,1′-bis-(diphenylphosphino)ferrocene]dichloropalladium(II), complex with dichloromethane (1.24 g) and potassium phosphate (32.2 g) at ambient temperature and the mixture was stirred at 100° C. for 60 hours. The mixture was evaporated in vacuo to remove 1,2-dimethoxyethane and the residue was dissolved in a mixture of ethyl acetate (600 mL) and water (300 mL). The separated organic layer was washed with brine, dried over magnesium sulfate, and evaporated in vacuo. The residue was purified by column chromatography on silica gel eluting with ethyl acetate to give 1-(phenylacetyl)-5-(4-pyridinyl)indoline (8.02 g) as a white powder.

後処理

  1. customThe mixture was evaporated in vacuo
  2. customto remove 1,2-dimethoxyethane
  3. dissolutionthe residue was dissolved in a mixture of ethyl acetate (600 mL) and water (300 mL)
  4. washThe separated organic layer was washed with brine
  5. dry with materialdried over magnesium sulfate
  6. customevaporated in vacuo
  7. customThe residue was purified by column chromatography on silica gel eluting with ethyl acetate

出典と根拠

ORDレコード
ord-ddba1c18feda415aba0fbfac60cffdf3
出典データセット
uspto-grants-2012_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08211919B2

反応ノート

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