Xanthone → HCID 23035018、化合物

HRID 1172030

反応式

HRID 1172030 の反応式
[C:1]1([S:7]([C:9]2[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=2)=O)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.[CH:15]1[C:28]2[C:27](=[O:29])[C:26]3[C:21](=[CH:22][CH:23]=[CH:24][CH:25]=3)[O:20][C:19]=2[CH:18]=[CH:17][CH:16]=1.[F:30][C:31]([F:44])([F:43])[S:32]([O:35]S(C(F)(F)F)(=O)=O)(=[O:34])=[O:33]>ClCCl>[F:30][C:31]([F:44])([F:43])[S:32]([O-:35])(=[O:34])=[O:33].[C:9]1([S+:7]([C:1]2[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=2)[C:16]2[CH:17]=[CH:18][C:19]3[O:20][C:21]4[C:26](=[CH:25][CH:24]=[CH:23][CH:22]=4)[C:27](=[O:29])[C:28]=3[CH:15]=2)[CH:10]=[CH:11][CH:12]=[CH:13][CH:14]=1

参加物

5

反応物 3

HCID 7020XanthoneHCID 13679Diphenyl sulfoxideHCID 67749Trifluoromethanesulfonic anhydride

生成物 1

HCID 23035018HCID 23035018、化合物収率 58%

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒

実験手順

To 320 ml of dichloromethane were dissolved 20.2 g (0.1 mol) of diphenylsulfoxide and 19.6 g (0.1 mol) of xanthene-9-one, and 28.2 g (0.1 mol) of trifluoromethanesulfonic anhydride was added dropwise thereto at −70 to −60° C., followed by gradually warming to room temperature and reacting with stirring for 4 hours. After completion of the reaction, the obtained reaction solution was washed with water (160 ml×4 times) and concentrated under reduced pressure, followed by purifying the obtained crude product with column chromatography to obtain 30.7 g of objective substance as pale brown glassy substance (yield: 58%).

後処理

  1. additionwas added dropwise
  2. customat −70 to −60° C.
  3. customAfter completion of the reaction
  4. customthe obtained reaction solution
  5. washwas washed with water (160 ml×4 times)
  6. concentrationconcentrated under reduced pressure
  7. customby purifying the
  8. customobtained crude product with column chromatography
  9. customto obtain 30.7 g of objective substance as pale brown glassy substance (yield: 58%)

出典と根拠

ORDレコード
ord-5c1a146f3f074c33bdca028c85aa986c
出典データセット
uspto-grants-2010_11
特許番号
US07833691B2

関連ノート

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