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Sodium Carbonate → HCID 22459291、化合物

HRID 355742
ノート
印刷プレビュー

反応式

HRID 355742 の反応式
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10](=[O:19])[C:11]2[CH:16]=[CH:15][C:14](Br)=[C:13]([CH3:18])[CH:12]=2)=[CH:5][C:4]=1[N:20]1[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]1.C(=O)([O-])[O-].[Na+].[Na+].[S:33]1[CH:37]=[CH:36][C:35](B(O)O)=[CH:34]1>O.COCCOC>[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([NH:9][C:10](=[O:19])[C:11]2[CH:16]=[CH:15][C:14]([C:35]3[CH:36]=[CH:37][S:33][CH:34]=3)=[C:13]([CH3:18])[CH:12]=2)=[CH:5][C:4]=1[N:20]1[CH2:25][CH2:24][N:23]([CH3:26])[CH2:22][CH2:21]1
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 3

HCID 10340Sodium CarbonateHCID 581760Thiophene-3-boronic acidHCID 117962574-Bromo-N-[4-methoxy-3-(4-methyl-1-piperazinyl)phenyl]-3-methylbenzamide

生成物 1

HCID 22459291HCID 22459291、化合物収率 68.3%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8071
1,2-Dimethoxyethane
溶媒

実験手順

N-(4Methoxy-3-(4-methyl-1-piperazinyl)phenyl)-4-bromo-3-methylbenzamide (0.35 g, 0.84 mmol), sodium carbonate (89 mg, 0.84 mmol), tetrakis (triphenylphosphine)palladium(0) (49 mg, 0.05 equiv), 3-thiophenyl boronic acid (115 mg, 0.84 mmol) in water (18 ml) and DME (18 ml) were heated at reflux under argon for 18 h. The solution was partitioned between saturated aqueous potassium carbonate solution (50 ml) and chloroform (50 ml), the organic extracts dried (sodium sulphate), filtered and evaporated to dryness under reduced pressure. The resulting oil was purified by column chromatography (silica, chloroform/methanol 5-30%) to afford the tide compound as an oil (242 mg, 63%) which was crystallised as an oxalate salt from methanol chloroform.

後処理

  1. temperatureat reflux under argon for 18 h
  2. customThe solution was partitioned between saturated aqueous potassium carbonate solution (50 ml) and chloroform (50 ml)
  3. dry with materialthe organic extracts dried (sodium sulphate)
  4. filtrationfiltered
  5. customevaporated to dryness under reduced pressure
  6. customThe resulting oil was purified by column chromatography (silica, chloroform/methanol 5-30%)

出典と根拠

ORDレコード
ord-f80a96c18a834c2286de3754b93e1321
出典データセット
uspto-grants-1998_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05834471

反応ノート

読み込み中…

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