Potassium hydride → HCID 178478936、化合物

HRID 1072699

反応式

HRID 1072699 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-:24].[Cl-]>C1COCC1>[Cl:22][Cr:23]([Cl:24])[C:14]1[CH:13]([C:11]2[CH:10]=[CH:9][CH:8]=[C:7]3[C:12]=2[N:3]=[CH:4][CH:5]=[CH:6]3)[C:21]2[C:16]([CH:15]=1)=[CH:17][CH:18]=[CH:19][CH:20]=2

参加物

5

反応物 3

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

生成物 1

HCID 178478936HCID 178478936、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) were suspended in 20 ml of THF and 0.3 g of 1-(8-quinolyl)indene (1.23 mol) were slowly added. The resultant violet suspension was stirred for three hours at room temperature and then added dropwise to a mixture of 0.46 g of chromium(III) chloride 3THF (1.23 mmol) in 50 ml of THF. Once this addition was complete the mixture was stirred for a further 16 hours. The solvent was removed in vacuo and the resultant solid extracted several times with hot toluene on a G4 frit. Once the solvent had been distilled off from the combined extracts the product was obtained as a green powder. This was washed several times with hexane and dried under HV, giving 0.22 g of dichloro[1-(8-quinolyl)indenyl]chromium(III) (50%).

後処理

  1. additionOnce this addition
  2. stirringwas stirred for a further 16 hours
  3. customThe solvent was removed in vacuo
  4. extractionthe resultant solid extracted several times with hot toluene on a G4 frit
  5. distillationOnce the solvent had been distilled off from the combined extracts the product
  6. customwas obtained as a green powder
  7. washThis was washed several times with hexane
  8. customdried under HV

出典と根拠

ORDレコード
ord-37a579a0376c4786b2fa160d02e264aa
出典データセット
uspto-grants-2005_06
特許番号
US06911516B1

関連ノート

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