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

Dimethyl Sulfoxide → 2-Bromo-9,9-dibutyl-9H-fluorene

HRID 1895759
ノート
印刷プレビュー

反応式

HRID 1895759 の反応式
C[C:2]([CH3:5])([O-])[CH3:3].[K+].[Br:7][C:8]1[CH:20]=[CH:19][C:18]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[CH2:11][C:10]=2[CH:9]=1.[CH2:21](I)[CH2:22][CH2:23][CH3:24].[CH3:26]S(C)=O>C(Cl)(Cl)Cl>[Br:7][C:8]1[CH:20]=[CH:19][C:18]2[C:17]3[C:12](=[CH:13][CH:14]=[CH:15][CH:16]=3)[C:11]([CH2:26][CH2:3][CH2:2][CH3:5])([CH2:21][CH2:22][CH2:23][CH3:24])[C:10]=2[CH:9]=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 679Dimethyl Sulfoxide2 回HCID 10962Butyl iodideHCID 143362-Bromo-9H-fluoreneHCID 23665647Potassium tert-butoxide

生成物 1

HCID 223816472-Bromo-9,9-dibutyl-9H-fluorene

試薬・触媒・溶媒 1

HCID 6212Chloroform溶媒

実験手順

Under a nitrogen atmosphere, to a solution obtained by dissolving 20.8 parts of potassium tert-butoxide in 102 parts of dimethylsulfoxide (DMSO), a solution obtained by dissolving 15.4 parts of 2-bromofluorene in 153 parts of dimethylsulfoxide (DMSO) was added dropwise. After stirring for 30 minutes, while keeping the reaction solution temperature to 40 to 45° C., 27.8 parts of butyl iodide was added dropwise. After stirring at 40° C. for 40 minutes, the reaction solution was added to ice water. The reaction mixture was extracted with chloroform-water, the chloroform phase was dried over magnesium sulfate, and then chloroform was distilled off to obtain a brown tarry solid. This brown tarry solid was dissolved in a small amount of chloroform, and separated and purified by column chromatography (hexane) to obtain 12.6 parts of 2-bromo-9,9-dibutylfluorene as a colorless crystal.

後処理

  1. customUnder a nitrogen atmosphere, to a solution obtained
  2. customa solution obtained
  3. additionwas added dropwise
  4. customto 40 to 45° C.
  5. stirringAfter stirring at 40° C. for 40 minutes
  6. extractionThe reaction mixture was extracted with chloroform-water
  7. dry with materialthe chloroform phase was dried over magnesium sulfate
  8. distillationchloroform was distilled off
  9. customto obtain a brown tarry solid
  10. customseparated
  11. custompurified by column chromatography (hexane)

出典と根拠

ORDレコード
ord-b8daf464d43342508dd127168c6cac59
出典データセット
uspto-grants-2013_08
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US08513520B2

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