Benzyltrimethylammonium hydroxide → HCID 86734504、化合物

HRID 596545

反応式

HRID 596545 の反応式
[CH:1]([C:3]1[CH:15]=[CH:14][C:13]2[C:12]3[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=3)[CH2:6][C:5]=2[CH:4]=1)=[CH2:2].[OH-:16].C([N+](C)(C)C)C1C=CC=CC=1>N1C=CC=CC=1>[CH:1]([C:3]1[C:4](=[O:16])[C:5]2[C:13](=[CH:14][CH:15]=1)[C:12]1[C:7](=[CH:8][CH:9]=[CH:10][CH:11]=1)[CH:6]=2)=[CH2:2]

参加物

4

反応物 2

HCID 66854Benzyltrimethylammonium hydroxideHCID 110416072-ethenyl-9H-fluorene

生成物 1

HCID 86734504HCID 86734504、化合物

試薬・触媒・溶媒 1

HCID 1049Pyridine溶媒2 回

反応条件

温度
0 °C

実験手順

The 2-vinylfluorene prepared in Example I is dissolved in 800 milliliters of pyridine and cooled to 0° C. One-half milliliter of a 40% solution of benzyltrimethyl ammonium hydroxide in pyridine is slowly added with air being bubbled through the reaction solution. The initially formed red coloration fades over a period of 1 to 2 hours and the solution is poured into water and extracted with benzene to yield 9 grams (90% theory) of a yellow solid. The residue is chromatographed on alumina (Woehlm basic) and eluted with benzene. Recrystallization from hexane gives 2-vinylfluorenone as a pale yellow material (melting point 69°-70° C). The structure of the product is confirmed by nuclear magnetic resonance and elemental analysis.

後処理

  1. custombeing bubbled through the reaction solution
  2. additionthe solution is poured into water
  3. extractionextracted with benzene
  4. customto yield 9 grams (90% theory) of a yellow solid
  5. customThe residue is chromatographed on alumina (Woehlm basic)
  6. washeluted with benzene
  7. customRecrystallization from hexane

出典と根拠

ORDレコード
ord-5050f0d7c04f41ca9cf04023d55c24f4
出典データセット
uspto-grants-1977_03
特許番号
US04011266

関連ノート

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