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Sodium Carbonate → HCID 18759616, 화합물

HRID 432554
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HRID 432554 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 10340Sodium CarbonateHCID 18759597HCID 18759597, 화합물2회HCID 18759599HCID 18759599, 화합물HCID 22242641Methanol--water (1/1)

생성물 1

HCID 18759616HCID 18759616, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

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온도
100 °C

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-b78f53c85c84454bbf8a957fb2d4eee3
출처 데이터셋
uspto-grants-2003_12
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06664111B2

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