Triphenylphosphine → 6-Chloro-2-[(4,6-dimethoxypyrimidin-2-yl)oxy]benzoic acid 4-pyridylthio ester

HRID 2396675

반응식

HRID 2396675 반응식
[Cl:1][C:2]1[C:7]([C:8]([OH:10])=[O:9])=[C:6]([O:11][C:12]2[N:17]=[C:16]([O:18][CH3:19])[CH:15]=[C:14]([O:20][CH3:21])[N:13]=2)[CH:5]=[CH:4][CH:3]=1.[CH:22]1[C:27]([S:28]C2C=CN=CC=2)=[CH:26][CH:25]=[N:24][CH:23]=1.C1(P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1>C1(C)C=CC=CC=1>[N:24]1[CH:25]=[CH:26][C:27]([S:28][O:9][C:8](=[O:10])[C:7]2[C:2]([Cl:1])=[CH:3][CH:4]=[CH:5][C:6]=2[O:11][C:12]2[N:13]=[C:14]([O:20][CH3:21])[CH:15]=[C:16]([O:18][CH3:19])[N:17]=2)=[CH:22][CH:23]=1

참가 물질

5

반응물 3

HCID 11776TriphenylphosphineHCID 6046504,4'-Dipyridyl SulfideHCID 156119442-Chloro-6-((4,6-dimethoxypyrimidin-2-yl)oxy)benzoic acid

생성물 1

HCID 543333746-Chloro-2-[(4,6-dimethoxypyrimidin-2-yl)oxy]benzoic acid 4-pyridylthio ester수율 90%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

31.0 g of 6-chloro-2-[(4,6-dimethoxypyrimidin-2-yl)oxy]benzoic acid, 22.0 g of 4,4'-dipyridylsulfide and 26.2 g of triphenylphosphine were suspended in 250 ml of toluene, and were violently stirred at room temperature for 2 hours. The reaction mixture was filtered, and the toluene was distilled off under reduced pressure. The residue thus obtained was purified by silica gel column chromatography to obtain 36.0 g of the above identified compound as a white crystal (yield 90%).

후처리

  1. filtrationThe reaction mixture was filtered
  2. distillationthe toluene was distilled off under reduced pressure
  3. customThe residue thus obtained
  4. customwas purified by silica gel column chromatography
  5. customto obtain 36.0 g of the

출처 및 근거

ORD 기록
ord-f24b90f1e2ae4c94b5aec90b4c1d5fe3
출처 데이터셋
uspto-grants-1996_02
특허 번호
US05494888

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