Diethyl Ether → HCID 22482395, 화합물

HRID 2181871노트

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HRID 2181871 반응식
[CH:1]1[C:14]2[C:5](=[N:6][CH:7]=[C:8]3[C:13]=2[CH:12]=[CH:11][CH:10]=[CH:9]3)[CH:4]=[CH:3][CH:2]=1.C[Li].[CH2:17](OCC)C.[CH3:22][O:23][C:24]1[CH:29]=[CH:28][C:27]([S:30](Cl)(=[O:32])=[O:31])=[CH:26][C:25]=1[C:34]([F:37])([F:36])[F:35]>>[CH3:22][O:23][C:24]1[CH:29]=[CH:28][C:27]([S:30]([N:6]2[CH:7]([CH3:17])[C:8]3[C:13](=[CH:12][CH:11]=[CH:10][CH:9]=3)[C:14]3[CH:1]=[CH:2][CH:3]=[CH:4][C:5]2=3)(=[O:32])=[O:31])=[CH:26][C:25]=1[C:34]([F:37])([F:36])[F:35]

참가 물질

5

반응물 4

HCID 3283Diethyl EtherHCID 9189PhenanthridineHCID 224823844-Methoxy-3-(trifluoromethyl)benzenesulfonyl chlorideHCID 178418348HCID 178418348, 화합물

생성물 1

HCID 22482395HCID 22482395, 화합물수율 44.2%

실험 절차

The title compound was prepared from phenanthridine (5.38 g, 30 mmol), 1.4 M methyllithium in diethyl ether (21.8 mL, 30.5 mmol), and 4-methoxy-3-(trifluoromethyl)benzenesulfonyl chloride (8.24 g, 30 mmol) according to the procedure and in the same manner as described in Example 1, step a. The crude product was purified by flash column chromatography on silica gel, eluting with a mixture of ethyl acetate-hexane (1:8) to yield 5-{[4-methoxy-3-(trifluoromethyl)phenyl]sulfonyl}-6-methyl-5,6-dihydrophenanthridine (5.75 g, 13.27 mmol, 44%) as a white solid;

후처리

  1. customThe crude product was purified by flash column chromatography on silica gel
  2. washeluting with a mixture of ethyl acetate-hexane (1:8)

출처 및 근거

ORD 기록
ord-4918139372c842118bdaf3df54ea6932
출처 데이터셋
uspto-grants-2005_05
특허 번호
US06894061B2

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