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

Hydrochloric Acid → 4'-Phenylthio-2,4-dihydroxybenzophenone

HRID 1369327
ノート
印刷プレビュー

反応式

HRID 1369327 の反応式
[OH:1][C:2]1[CH:16]=[C:15]([OH:17])[CH:14]=[CH:13][C:3]=1[C:4]([C:6]1[CH:11]=[CH:10][C:9](Cl)=[CH:8][CH:7]=1)=[O:5].[C:18]1([SH:24])[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1.C(=O)([O-])[O-].[K+].[K+].Cl>CN1CCCC1=O>[C:18]1([S:24][C:9]2[CH:10]=[CH:11][C:6]([C:4](=[O:5])[C:3]3[CH:13]=[CH:14][C:15]([OH:17])=[CH:16][C:2]=3[OH:1])=[CH:7][CH:8]=2)[CH:23]=[CH:22][CH:21]=[CH:20][CH:19]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

HCID 313Hydrochloric AcidHCID 7969ThiophenolHCID 11430Potassium CarbonateHCID 519532(4-Chlorophenyl)(2,4-dihydroxyphenyl)methanone

生成物 1

HCID 120842914'-Phenylthio-2,4-dihydroxybenzophenone収率 42.8%

試薬・触媒・溶媒 1

HCID 13387N-methyl-2-pyrrolidone
溶媒

実験手順

A mixture of 39 g (156 mmol) of 2,4-dihydroxy-4′-chlorobenzophenone, 22.4 g (204 mmol) of thiophenol and 26 g (188 mmol) of potassium carbonate is stirred in 300 ml of N-methyl-2-pyrrolidone for 24 hours at a temperature of 210° C. After cooling the reaction mixture is neutralized with hydrochloric acid (10%) and extracted with 4×250 ml of ethyl acetate. The solution so obtained is washed with water and afterwards with a saturated solution of sodium chloride. The residue which is obtained, after drying over anhydrous magnesium sulfate, filtration and evaporation of the solvent is subjected to chromatography on silica gel (ethyl acetate/hexane 1:5). The product is recrystallized from ethyl acetate/hexane. 21.5 g of the compound are obtained as yellow crystals with a melting point of 117-118° C.

後処理

  1. temperatureAfter cooling the reaction mixture
  2. extractionextracted with 4×250 ml of ethyl acetate
  3. customThe solution so obtained
  4. washis washed with water and afterwards with a saturated solution of sodium chloride
  5. customThe residue which is obtained
  6. dry with materialafter drying over anhydrous magnesium sulfate, filtration and evaporation of the solvent
  7. customThe product is recrystallized from ethyl acetate/hexane

出典と根拠

ORDレコード
ord-b01ce4f9e27840cbb632a703bbf82d46
出典データセット
uspto-grants-2003_06
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06576797B1

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