Aluminum sec-butoxide → HCID 21977175、化合物

HRID 488979

反応式

HRID 488979 の反応式
[F:1][C:2]1[CH:23]=[CH:22][C:21]2[C:20](=O)[C:19]3[C:6](=[CH:7][C:8]4[C:9](=O)[C:10]5[C:15]([C:16](=O)[C:17]=4[CH:18]=3)=[CH:14][C:13]([F:26])=[CH:12][CH:11]=5)[C:5](=O)[C:4]=2[CH:3]=1.CC(CC)[O-].CC(CC)[O-].CC(CC)[O-].[Al+3]>C1(O)CCCCC1>[F:1][C:2]1[CH:23]=[CH:22][C:21]2[C:4](=[CH:5][C:6]3[C:19]([CH:20]=2)=[CH:18][C:17]2[C:8](=[CH:9][C:10]4[C:15]([CH:16]=2)=[CH:14][C:13]([F:26])=[CH:12][CH:11]=4)[CH:7]=3)[CH:3]=1

参加物

4

反応物 2

HCID 61289Aluminum sec-butoxideHCID 22269481HCID 22269481、化合物

生成物 1

HCID 21977175HCID 21977175、化合物

試薬・触媒・溶媒 1

HCID 7966Cyclohexanol溶媒

反応条件

温度
100 °C

実験手順

To a mixture of 0.5 grams of 2,9-difluoropentacene-5,7,12,14-tetrone and 20 mL of cyclohexanol in a flask was added 3.640 grams of aluminum tri(sec-butoxide). The mixture was heated at 100° C. for approximately 12 hours and a blue solid deposited on the sides of the flask. The reaction mixture was centrifuged and the blue solid residue was washed with cyclohexanol, centrifuged twice, and then washed with acetone and collected by filtration. This solid was washed with 50% concentrated HCl and the resulting mixture was centrifuged to give a blue solid. This solid was washed with THF and collected by centrifugation to give 2,9-difluoropentacene.

後処理

  1. washthe blue solid residue was washed with cyclohexanol
  2. washwashed with acetone
  3. filtrationcollected by filtration
  4. washThis solid was washed with 50% concentrated HCl
  5. customto give a blue solid
  6. washThis solid was washed with THF
  7. customcollected by centrifugation

出典と根拠

ORDレコード
ord-1ba33c954a2644949732b83de0338089
出典データセット
uspto-grants-2005_12
特許番号
US06974877B2

関連ノート

読み込み中…