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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
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2-Chloro-1,4-naphthoquinone → 1,4-Naphthalenedione, 2-chloro-3-[cis-4-(4-chlorophenyl)cyclohexyl]-

HRID 129024
ノート
印刷プレビュー

反応式

HRID 129024 の反応式
[Cl:1][C:2]1[C:3](=[O:13])[C:4]2[C:9]([C:10](=[O:12])[CH:11]=1)=[CH:8][CH:7]=[CH:6][CH:5]=2.[Cl:14][C:15]1[CH:20]=[CH:19][C:18]([CH:21]2[CH2:26][CH2:25][CH:24](C(O)=O)[CH2:23][CH2:22]2)=[CH:17][CH:16]=1.S(OOS([O-])(=O)=O)([O-])(=O)=O.[NH4+].[NH4+]>C(#N)C.O.[N+]([O-])([O-])=O.[Ag+]>[Cl:14][C:15]1[CH:20]=[CH:19][C:18]([CH:21]2[CH2:26][CH2:25][CH:24]([C:11]3[C:10](=[O:12])[C:9]4[C:4]([C:3](=[O:13])[C:2]=3[Cl:1])=[CH:5][CH:6]=[CH:7][CH:8]=4)[CH2:23][CH2:22]2)=[CH:17][CH:16]=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 138912-Chloro-1,4-naphthoquinoneHCID 62648Ammonium PersulfateHCID 27357924-(4-Chlorophenyl)cyclohexane-1-carboxylic acid

生成物 1

HCID 111010701,4-Naphthalenedione, 2-chloro-3-[cis-4-(4-chlorophenyl)cyclohexyl]-収率 35%

試薬・触媒・溶媒 3

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

実験手順

A mixture of 2-chloro-1,4-naphthoquinone (3.95 g, 0.02 mol), 4-(4-chlorophenyl)cyclohexane-1-carboxylic acid (4.9 g, 0.02 mol) and powdered silver nitrate (1.05 g, 0.0062 mol) was heated to reflux with vigorous stirring in 40 ml of acetonitrile. A solution of ammonium persulphate (12.0 g, 0.0525 mol) in 50 ml of water was added dropwise over 1 hour. The mixture was refluxed for 3 hours then cooled in ice for 30 mins, after which it was filtered, and the residual sticky solid extracted twice with boiling chloroform to remove inorganic material. The chloroform was removed by evaporation to leave a yellow-brown solid (ca 2.7 g). This was dissolved in 40 ml of boiling acetonitrile; a little insoluble material was removed by filtration. On cooling, the title compound separated as yellow crystals, (550 mg) m.p. 172°-175° C.

後処理

  1. temperaturewas heated
  2. temperatureto reflux
  3. temperatureThe mixture was refluxed for 3 hours
  4. temperaturethen cooled in ice for 30 mins
  5. filtrationafter which it was filtered
  6. extractionthe residual sticky solid extracted twice with boiling chloroform
  7. customto remove inorganic material
  8. customThe chloroform was removed by evaporation

出典と根拠

ORDレコード
ord-076d551d4ea741cba8afc23e379a8905
出典データセット
uspto-grants-1995_11
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05466711

反応ノート

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