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Sodium Carbonate → 5-(3,5-dichlorophenyl)-1H-indole-2-carboxylic acid ethyl ester

HRID 646168
ノート
印刷プレビュー

反応式

HRID 646168 の反応式
[CH2:1]([O:3][C:4]([C:6]1[NH:7][C:8]2[C:13]([C:14]=1Cl)=[CH:12][C:11](Br)=[CH:10][CH:9]=2)=[O:5])[CH3:2].[Cl:17][C:18]1[CH:19]=[C:20](B(O)O)[CH:21]=[C:22]([Cl:24])[CH:23]=1.C1C=CC(P(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1.C([O-])([O-])=O.[Na+].[Na+]>CC#N.CC(O)C.O.CC([O-])=O.CC([O-])=O.[Pd+2]>[CH2:1]([O:3][C:4]([C:6]1[NH:7][C:8]2[C:13]([CH:14]=1)=[CH:12][C:11]([C:20]1[CH:19]=[C:18]([Cl:17])[CH:23]=[C:22]([Cl:24])[CH:21]=1)=[CH:10][CH:9]=2)=[O:5])[CH3:2]
参加物実験手順後処理出典と根拠反応ノート

参加物

9

反応物 4

HCID 10340Sodium CarbonateHCID 11776TriphenylphosphineHCID 27343313,5-Dichlorophenylboronic acidHCID 28330549ethyl 5-bromo-3-chloro-1H-indole-2-carboxylate

生成物 1

HCID 686972085-(3,5-dichlorophenyl)-1H-indole-2-carboxylic acid ethyl ester収率 69.2%

試薬・触媒・溶媒 4

HCID 167845
palladium(II) acetate
触媒
HCID 962Water溶媒
HCID 3776Isopropanol溶媒
HCID 6342Acetonitrile溶媒

実験手順

To a stirred solution of 5-bromo-3-chloro-1H-indole-2-carboxylic acid ethyl ester (500 mg, 1.86 mmol) and 3,5-dichlorophenyl boronic acid (530 mg, 2.78 mmol) in a mixture of MeCN (26 mL) and i-PrOH (3.3 mL) at room temperature under argon, was added Pd(OAc)2 (12 mg, 0.05 mmol), Ph3P (40 mg, 0.15 mmol) and Na2CO3 (2M aq., 16 mL) and the resulting mixture was heated at reflux for 3 h. After cooling to room temperature the reaction was diluted with water (20 mL) and extracted with EtOAc (3×30 mL). The combined organic extracts were washed with water, brine and dried (MgSO4). Solvent removal and purification by chromatography afforded the sub-title compound (430 mg, 69%).

後処理

  1. temperaturethe resulting mixture was heated
  2. temperatureat reflux for 3 h
  3. extractionextracted with EtOAc (3×30 mL)
  4. washThe combined organic extracts were washed with water, brine
  5. dry with materialdried (MgSO4)
  6. customSolvent removal and purification by chromatography

出典と根拠

ORDレコード
ord-355bf65a6dc247d8a6a2db493828223c
出典データセット
uspto-grants-2010_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07705023B2

反応ノート

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