1,2-Dimethoxyethane → HCID 57930925, 화합물

HRID 1096947노트

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HRID 1096947 반응식
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:10]=[C:11](OS(C(F)(F)F)(=O)=O)[CH:12]=1)[C:6]([O:8][CH3:9])=[O:7].[NH:21]1[C:29]2[C:24](=[CH:25][C:26](B(O)O)=[CH:27][CH:28]=2)[CH:23]=[CH:22]1.P([O-])([O-])([O-])=O.[K+].[K+].[K+].COCCOC>C(OCC)(=O)C.C1C=CC([P]([Pd]([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)([P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)[P](C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)(C2C=CC=CC=2)C2C=CC=CC=2)=CC=1>[NH:21]1[C:29]2[C:24](=[CH:25][C:26]([C:11]3[CH:10]=[C:5]([CH:4]=[C:3]([O:2][CH3:1])[CH:12]=3)[C:6]([O:8][CH3:9])=[O:7])=[CH:27][CH:28]=2)[CH:23]=[CH:22]1

참가 물질

7

반응물 4

HCID 80711,2-DimethoxyethaneHCID 62657Potassium Phosphate, TribasicHCID 27343615-Indolylboronic acidHCID 54576351HCID 54576351, 화합물

생성물 1

HCID 57930925HCID 57930925, 화합물

시약·촉매·용매 2

HCID 178418397HCID 178418397, 화합물촉매HCID 8857Ethyl Acetate용매

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온도
85 °C

실험 절차

A mixture of methyl 3-methoxy-5-trifluoromethanesulfonyloxybenzoate (314 mg, 1.00 mmol), 5-indoleboronic acid (193 mg, 1.20 mmol), tetrakis(triphenylphosphine)palladium(0) (57.8 mg, 0.050 mmol), potassium phosphate (318 mg, 1.50 mmol) and 1,2-dimethoxyethane (5.0 ml) was stirred in a nitrogen atmosphere at 85° C. for 13 hours. After left cooled, the reaction mixture was diluted with ethyl acetate, filtered through Celite, and the filtrate was concentrated under reduced pressure. The residue was purified through silica gel column chromatography to obtain the title compound as a colorless oil.

후처리

  1. waitAfter left
  2. temperaturecooled
  3. filtrationfiltered through Celite
  4. concentrationthe filtrate was concentrated under reduced pressure
  5. customThe residue was purified through silica gel column chromatography

출처 및 근거

ORD 기록
ord-3bb68a63e7384df9ab70ebb4fb4d500c
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08138197B2

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