Potassium Phosphate, Tribasic → HCID 23157344, 화합물

HRID 507978노트

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HRID 507978 반응식
FC(F)(F)S(O[C:7]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:8]=1[CH2:9][CH2:10][C:11]2=[O:16])(=O)=O.[CH3:19][C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[C:21]=1B(O)O.P([O-])([O-])([O-])=O.[K+].[K+].[K+]>C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd].C1(P(C2CCCCC2)C2C=CC=CC=2C2C=CC=CC=2)CCCCC1.C1(C)C=CC=CC=1>[CH3:19][C:20]1[CH:25]=[CH:24][CH:23]=[C:22]([CH3:26])[C:21]=1[C:7]1[CH:15]=[CH:14][CH:13]=[C:12]2[C:8]=1[CH2:9][CH2:10][C:11]2=[O:16]

참가 물질

7

반응물 3

HCID 62657Potassium Phosphate, TribasicHCID 5833222,6-Dimethylphenylboronic acidHCID 218380021-Oxo-2,3-dihydro-1H-inden-4-yl trifluoromethanesulfonate

생성물 1

HCID 23157344HCID 23157344, 화합물수율 85.5%

시약·촉매·용매 3

HCID 27342162-(Dicyclohexylphosphino)biphenyl촉매HCID 9811564Bis(dibenzylideneacetone)palladium촉매HCID 1140Toluene용매

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온도
90 °C

실험 절차

A mixture of 1-oxo-2,3-dihydro-1H-inden-4-yl trifluoromethanesulfonate (10.0 g, 35.7 mmol), 2,6-dimethylphenylboronic acid (6.96 g, 46.4 mmol), 2-(dicyclohexylphosphino)biphenyl (750 mg, 2.14 mmol), tris(dibenzylideneacetone)dipalladium(0) (1.31 mg, 1.43 mmol), tripotassium phosphate (15.2 g, 71.4 mmol) and toluene (200 mL) was heated under reflux under an argon atmosphere at 90° C. for 16 hr. After cooling the reaction mixture, the insoluble material was filtered off, and the filtrate was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (5%-45% ethyl acetate/hexane) to give the title compound (7.21 g, yield 85%) as pale-yellow crystals.

후처리

  1. temperaturewas heated
  2. temperatureAfter cooling the reaction mixture
  3. filtrationthe insoluble material was filtered off
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified by silica gel column chromatography (5%-45% ethyl acetate/hexane)

출처 및 근거

ORD 기록
ord-abf8d35e7cc94dea9775d44c982f1409
출처 데이터셋
uspto-grants-2010_08
특허 번호
US07786165B2

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