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Triphenylphosphine → 6-Trimethylsilylethynyl-8-(3-nitrophenyl)-1,7-naphthyridine

HRID 369031
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HRID 369031 반응식
FC(F)(F)S(O[C:7]1[CH:8]=[C:9]2[C:14](=[C:15]([C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([N+:23]([O-:25])=[O:24])[CH:18]=3)[N:16]=1)[N:13]=[CH:12][CH:11]=[CH:10]2)(=O)=O.[C:28]([Si:30]([CH3:33])([CH3:32])[CH3:31])#[CH:29].C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>CN(C)C=O.C(N(CC)CC)C.C(OCC)(=O)C.[Cu](I)I>[CH3:31][Si:30]([C:28]#[C:29][C:7]1[CH:8]=[C:9]2[C:14](=[C:15]([C:17]3[CH:22]=[CH:21][CH:20]=[C:19]([N+:23]([O-:25])=[O:24])[CH:18]=3)[N:16]=1)[N:13]=[CH:12][CH:11]=[CH:10]2)([CH3:33])[CH3:32]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

8

반응물 3

HCID 11776TriphenylphosphineHCID 66111TrimethylsilylacetyleneHCID 108109346-Trifluoromethylsulfonyloxy-8-(3-nitrophenyl)-1,7-naphthyridine

생성물 1

HCID 232846376-Trimethylsilylethynyl-8-(3-nitrophenyl)-1,7-naphthyridine

시약·촉매·용매 4

HCID 83717Copper iodide촉매
HCID 6228
Dimethylformamide
용매
HCID 8471Triethylamine용매
HCID 8857Ethyl Acetate용매

실험 절차

To a solution of 6-trifluoromethylsulfonyloxy-8-(3-nitrophenyl)-1,7-naphthyridine (200 mg, 0.50 mmol; prepared according to example 13) in dimethylformamide (1 ml) and triethylamine (0.5 ml) is added ethynyltrimethylsilane (0.078 ml, 0.56 mmol), bis(dibensylideneacetone)palladium (5.8 mg, 0.020 mmol), triphenylphosphine (5.3 mg, 0.020 mmol) and copper iodide (3.8 mg, 0.020 mmol). The mixture is kept at 60° C. for 2 h. The solution is diluted with ethyl acetate and washed with water. The product is purified by flash column chromatography on silica gel (20:0.2 toluene/acetone) affording 6-trimethylsilylethynyl-8-(3-nitrophenyl)-1,7-naphthyridine. (Mass M+H 348; mp 160-163° C.)

후처리

  1. washwashed with water
  2. customThe product is purified by flash column chromatography on silica gel (20:0.2 toluene/acetone)

출처 및 근거

ORD 기록
ord-461c80cb2d6143afb7cffdcfb39eef8e
출처 데이터셋
uspto-grants-2000_10
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06136821

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