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Sodium Carbonate → HCID 18759616、化合物

HRID 432554
ノート
印刷プレビュー

反応式

HRID 432554 の反応式
[CH2:1]([Si:4]([CH2:18][CH:19]=[CH2:20])([CH3:17])[CH2:5][CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11](B(O)O)=[CH:10][CH:9]=1)[CH:2]=[CH2:3].Br[C:22]1[C:35]2[C:26](=[C:27]3[C:32](=[CH:33][CH:34]=2)[C:31]([C:36]2[CH:41]=[CH:40][CH:39]=[CH:38][CH:37]=2)=[CH:30][CH:29]=[N:28]3)[N:25]=[CH:24][CH:23]=1.C([O-])([O-])=O.[Na+].[Na+].O.CO>C1(C)C=CC=CC=1>[CH2:1]([Si:4]([CH2:18][CH:19]=[CH2:20])([CH3:17])[CH2:5][CH2:6][CH2:7][C:8]1[CH:13]=[CH:12][C:11]([C:22]2[C:35]3[C:26](=[C:27]4[C:32](=[CH:33][CH:34]=3)[C:31]([C:36]3[CH:37]=[CH:38][CH:39]=[CH:40][CH:41]=3)=[CH:30][CH:29]=[N:28]4)[N:25]=[CH:24][CH:23]=2)=[CH:10][CH:9]=1)[CH:2]=[CH2:3]
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

6

反応物 4

HCID 10340Sodium CarbonateHCID 18759597HCID 18759597、化合物2 回HCID 18759599HCID 18759599、化合物HCID 22242641Methanol--water (1/1)

生成物 1

HCID 18759616HCID 18759616、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

反応条件

温度
100 °C

実験手順

4-{3-[diallyl(methyl)silyl]propyl}phenylboronic acid is made by the method of Casado and Stobart (Casado, M. A.; Stobart, S. R., Org. Lett., 2 (11), 2000, 1549-1552). 4-{3-[diallyl(methyl)silyl]propyl}phenylboronic acid (0.576 g) and a solution of Pd(Ph3)4 (58 mg) in 5 mL of degassed toluene is placed in a 50 mL Schlenk tube. The mixture is purged with nitrogen, after which a solution of 4-bromo-7-phenyl-1,10-phenanthroline (0.670 g) and Na2CO3 (428 mg, 4 mmol) in 5 mL of degassed 4:1 H2O/CH3OH is added. The mixture is heated under nitrogen at 100° C. with rapid stirring until TLC monitoring shows the reaction to be complete (ca 24 hrs). The reaction mixture is then added to a separatory funnel and washed with ether (3×50 mL). The combined organic fractions are dried over MgSO4 and concentrated by roto-evaporation. The desired product is purified by column chromatography on silica gel using a mixture of ethyl acetate and hexane.

後処理

  1. customThe mixture is purged with nitrogen
  2. additionis added
  3. customthe reaction
  4. custom(ca 24 hrs)
  5. additionThe reaction mixture is then added to a separatory funnel
  6. washwashed with ether (3×50 mL)
  7. dry with materialThe combined organic fractions are dried over MgSO4
  8. concentrationconcentrated by roto-evaporation
  9. customThe desired product is purified by column chromatography on silica gel using
  10. additiona mixture of ethyl acetate and hexane

出典と根拠

ORDレコード
ord-b78f53c85c84454bbf8a957fb2d4eee3
出典データセット
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06664111B2

反応ノート

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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