Hydrochloric Acid → HCID 11460950、化合物

HRID 488980

反応式

HRID 488980 の反応式
CC(CC)[O-].CC(CC)[O-].CC(CC)[O-].[Al+3].C1(O)CCCCC1.[CH3:24][C:25]1[CH:26]=[CH:27][C:28]2[CH:29]=[C:30]3[C:43]([C:44](=O)[C:45]=2[CH:46]=1)=[CH:42][C:41]1[C:32]([C:33](=O)[C:34]2[C:39]([CH:40]=1)=[CH:38][CH:37]=[C:36]([CH3:48])[CH:35]=2)=[CH:31]3.Cl>C1COCC1.CC(C)=O>[CH3:24][C:25]1[CH:26]=[CH:27][C:28]2[C:45](=[CH:44][C:43]3[C:30]([CH:29]=2)=[CH:31][C:32]2[C:41](=[CH:40][C:39]4[C:34]([CH:33]=2)=[CH:35][C:36]([CH3:48])=[CH:37][CH:38]=4)[CH:42]=3)[CH:46]=1

参加物

7

反応物 4

HCID 313Hydrochloric Acid2 回HCID 7966CyclohexanolHCID 61289Aluminum sec-butoxideHCID 22269443HCID 22269443、化合物

生成物 1

HCID 11460950HCID 11460950、化合物

試薬・触媒・溶媒 2

HCID 180Acetone溶媒HCID 8028Tetrahydrofuran溶媒

反応条件

温度
145 °C

実験手順

To a 500 mL three necked round bottom flask with a thermometer, and a distillation head was added 32.76 grams of aluminum tri(sec-butoxide) and 200 mLs of cyclohexanol. To this was added 9 grams 3,10-Dimethylpentacene-5,12-dione. The reaction mixture was heated to 145° C. At 140° C., 8.7 grams of a distillate was collected. The reaction mixture was heated at 140° C. for 43 hours and cooled to room temperature. A solid was isolated by centrifugation. The supernate liquid was poured off and the solid was slurried with 140 mLs of 1N HCl and isolated on a Buchner funnel. The solid was slurried three times with 100 mLs each 1N HCl and the solvent was poured off each time. The solid was slurried three times with 100 mLs of acetone and isolated by filtration. The solid was slurried three times with 100 mLs of THF and isolated by filtration. The residue was air dried to give 2,9-dimethylpentacene.

後処理

  1. distillationAt 140° C., 8.7 grams of a distillate was collected
  2. temperatureThe reaction mixture was heated at 140° C. for 43 hours
  3. temperaturecooled to room temperature
  4. customA solid was isolated by centrifugation
  5. additionThe supernate liquid was poured off
  6. customisolated on a Buchner funnel
  7. additionthe solvent was poured off each time
  8. customisolated by filtration
  9. customisolated by filtration
  10. customdried

出典と根拠

ORDレコード
ord-f284e0ee4ae84db88b9349c17cf1dbc0
出典データセット
uspto-grants-2005_12
特許番号
US06974877B2

関連ノート

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