Potassium hydride → HCID 178478635、化合物

HRID 1005642ノート

反応式

HRID 1005642 の反応式
[H-].[K+].[N:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[CH:13]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=[CH:14]2)[CH:6]=[CH:5][CH:4]=1.[Cl-:22].[Cr+3:23].[Cl-].[Cl-]>C1COCC1>[Cl-:22].[Cl-:22].[N:3]1[C:12]2[C:7](=[CH:8][CH:9]=[CH:10][C:11]=2[CH:13]2[C:21]3[C:16](=[CH:17][CH:18]=[CH:19][CH:20]=3)[CH:15]=[C:14]2[Cr+2:23])[CH:6]=[CH:5][CH:4]=1

参加物

5

反応物 3

HCID 82127Potassium hydrideHCID 6452300Chromium(3+) trichlorideHCID 219779971-(8-Quinolyl)indene

生成物 1

HCID 178478635HCID 178478635、化合物収率 50%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒2 回

実験手順

0.05 g of potassium hydride (1.23 mmol) was suspended in 20 ml of THF, and 0.3 g of 1-(8-quinolyl)indene (1.23 mmol) was slowly added. The resultant violet suspension was stirred at room temperature for three hours and then added dropwise to a mixture of 0.46 g of chromium(III)chloride 3THF (1.23 mmol) in 50 ml of THF and, when the addition was complete, the mixture was stirred for a further 16 hours. The solvent was removed under reduced presssure, and the resultant solid was extracted with hot toluene. After the solvent had been distilled off from the combined extracts, the product was obtained as a green powder, which was washed a number of times with hexane and dried under a high vacuum, giving 0.22 g of 1-(8-quinolyl)indenylchromium(III) dichloride (50%).

後処理

  1. additionwhen the addition
  2. stirringthe mixture was stirred for a further 16 hours
  3. customThe solvent was removed
  4. extractionthe resultant solid was extracted with hot toluene
  5. distillationAfter the solvent had been distilled off from the combined extracts
  6. customthe product was obtained as a green powder, which
  7. washwas washed a number of times with hexane
  8. customdried under a high vacuum

出典と根拠

ORDレコード
ord-d83e131eda6843e1a65b2df3e6fe8433
出典データセット
uspto-grants-2004_09
特許番号
US06787498B2

反応ノート

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