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Dichlone → HCID 178516332、化合物

HRID 2061944
ノート
印刷プレビュー

反応式

HRID 2061944 の反応式
Cl[C:2]1[C:3](=[O:14])[C:4]2[C:9]([C:10](=[O:13])[C:11]=1[Cl:12])=[CH:8][CH:7]=[CH:6][CH:5]=2.[Cl:15][C:16]1[CH:21]=[CH:20][C:19]([CH:22]2[CH2:27][CH2:26][CH:25](C(O)=O)[CH2:24][CH2:23]2)=[CH:18][CH:17]=1.S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+]>C(#N)C.O.[N+]([O-])([O-])=O.[Ag+]>[Cl:15][C:16]1[CH:21]=[CH:20][C:19]([C@H:22]2[CH2:27][CH2:26][C@H:25]([C:2]3[C:3](=[O:14])[C:4]4[C:9]([C:10](=[O:13])[C:11]=3[Cl:12])=[CH:8][CH:7]=[CH:6][CH:5]=4)[CH2:24][CH2:23]2)=[CH:18][CH:17]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 3

HCID 8342DichloneHCID 62648Ammonium PersulfateHCID 27357924-(4-Chlorophenyl)cyclohexane-1-carboxylic acid

生成物 1

HCID 178516332HCID 178516332、化合物収率 39.8%

試薬・触媒・溶媒 3

HCID 24470Silver Nitrate触媒HCID 962Water
溶媒
HCID 6342Acetonitrile溶媒

実験手順

A mixture of 2,3-dichloro-1,4-naphthoquinone (57.0 gm), 4-(4-chlorophenyl)-cyclohexane-1-carboxylic acid (60.0 gm) and silver nitrate (42.7 gm) is taken in acetonitrile (600 ml) and then a solution of ammonium persulphate (180.12 gm) in water (780 ml) is added. The mixture is heated to reflux, maintaining good stirring. The mixture was refluxed for 4 hrs. Then cooled in ice for about 1 hr after which it is filtered. The filtrate is kept aside for acetonitrile recovery. The solid is extracted with hot methylene chloride (100 ml×3). The inorganic salt is collected separately for recovery of silver. The organic layer is dried over anhydrous sodium sulphate and concentrated to get light brownish yellow solid (38.5 gm).

後処理

  1. temperatureThe mixture is heated
  2. temperatureto reflux
  3. temperaturemaintaining good stirring
  4. temperatureThe mixture was refluxed for 4 hrs
  5. temperatureThen cooled in ice for about 1 hr after which it
  6. filtrationis filtered
  7. extractionThe solid is extracted with hot methylene chloride (100 ml×3)
  8. customThe inorganic salt is collected separately for recovery of silver
  9. dry with materialThe organic layer is dried over anhydrous sodium sulphate
  10. concentrationconcentrated

出典と根拠

ORDレコード
ord-734842e13652449a97843cf9ccbad59d
出典データセット
uspto-grants-2012_10
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08283499B2

反応ノート

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