ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Dichlone → HCID 178516332、化合物

HRID 2061943
ノート
印刷プレビュー

反応式

HRID 2061943 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]([C@H:22]2[CH2:27][CH2:26][C@H: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 178525693HCID 178525693、化合物

生成物 1

HCID 178516332HCID 178516332、化合物収率 17.7%

試薬・触媒・溶媒 3

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

実験手順

A mixture of 2,3-dichloro-1,4-naphthoquinone (5 gm), trans 4-(4-chlorophenyl)-cyclohexane-1-carboxylic acid (6.06 gm) and silver nitrate (2.47 gm) is taken in acetonitrile (60 ml) and the mixture is heated to reflux, maintaining good stirring. Then a solution of ammonium persulphate (14.23 gm) in water (77 ml) is added through a dropping funnel over a period of 1-2 hrs. The mixture refluxed for 4 hrs. Then it is cooled in ice for about 1 hr after which it is filtered. The solid is extracted with hot methylene chloride (100 ml×3). The organic layer is dried over anhydrous sodium sulphate and concentrated to get light brownish yellow solid. This on crystallization from acetonitrile afforded the trans compound as yellow crystals (1.5 gm).

後処理

  1. temperaturethe mixture is heated
  2. temperatureto reflux
  3. temperaturemaintaining good stirring
  4. temperatureThe mixture refluxed for 4 hrs
  5. temperatureThen it is 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. dry with materialThe organic layer is dried over anhydrous sodium sulphate
  9. concentrationconcentrated
  10. customto get light brownish yellow solid
  11. customThis on crystallization from acetonitrile

出典と根拠

ORDレコード
ord-a047abe9920248ad859df6329d594396
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

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート