Potassium hydride → HCID 178478936, 화합물

HRID 1072699

반응식

HRID 1072699 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 178478936HCID 178478936, 화합물수율 50%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매2회

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-37a579a0376c4786b2fa160d02e264aa
출처 데이터셋
uspto-grants-2005_06
특허 번호
US06911516B1

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