Toluene → HCID 178420721、化合物

HRID 1198314ノート

反応式

HRID 1198314 の反応式
[CH2:1]([Li])[CH2:2][CH2:3][CH3:4].[CH3:6][CH2:7][CH2:8][CH2:9][CH2:10][CH3:11].[C:12]1([C:18]2[CH2:22][CH:21]=[C:20]([C:23]3[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=3)[CH:19]=2)[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1.[Cl-:29].[Cl-].[Cl-].[Cl-].[Zr+4:33].[C:34]1([CH3:40])[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=1>O1CCCC1>[Cl-:29].[Cl-:29].[C:8]1([C:2]2([Zr+2:33][C:20]3([C:23]4[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=4)[CH:21]=[CH:22][C:18]([C:12]4[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=4)=[CH:19]3)[CH:3]=[CH:4][C:40]([C:34]3[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=3)=[CH:1]2)[CH:7]=[CH:6][CH:11]=[CH:10][CH:9]=1

参加物

7

反応物 5

HCID 1140TolueneHCID 8058HexaneHCID 9856075Zirconium chloride (ZrCl4), (T-4)-HCID 12724477HCID 12724477、化合物HCID 178418339Butyllithium

生成物 1

HCID 178420721HCID 178420721、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

反応条件

温度
-20 °C

実験手順

A solution (1.4 ml) of n-butyllithium in hexane (1.6 mole/liter, 0.0023 mole n-butyllithium) at 80° C. was added slowly to 0.50 g (0.0023 mole) of 1,3-diphenylcyclopentadiene dissolved in 20 ml tetrahydrofuran. The mixture thus obtained was allowed to reach room temperature. A mixture of 0.268 g (0.00115 mole) of zirconium tetrachloride in 10 ml tetrahydrofuran was slowly added. After stirring the mixture for two hours, the solvents were evaporated. The solid material obtained was taken up in toluene and centrifuged. The supernatant was decanted and cooled to -20° C. The crystallized product was recovered by filtration.

後処理

  1. customThe mixture thus obtained
  2. customto reach room temperature
  3. additionwas slowly added
  4. customthe solvents were evaporated
  5. customThe solid material obtained
  6. customThe supernatant was decanted
  7. filtrationThe crystallized product was recovered by filtration

出典と根拠

ORDレコード
ord-6a9d3bf2deec470c99d9fc1505ecd6f0
出典データセット
uspto-grants-1994_01
特許番号
US05279999

反応ノート

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