Diethyl Ether → HCID 22482395、化合物

HRID 2181871ノート

反応式

HRID 2181871 の反応式
[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]

参加物

5

反応物 4

HCID 3283Diethyl EtherHCID 9189PhenanthridineHCID 224823844-Methoxy-3-(trifluoromethyl)benzenesulfonyl chlorideHCID 178418348HCID 178418348、化合物

生成物 1

HCID 22482395HCID 22482395、化合物収率 44.2%

実験手順

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;

後処理

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

出典と根拠

ORDレコード
ord-4918139372c842118bdaf3df54ea6932
出典データセット
uspto-grants-2005_05
特許番号
US06894061B2

反応ノート

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