Toluene → Cobalt (II) acetylacetonate

HRID 1722498

반응식

HRID 1722498 반응식
[CH3:1][C:2]([CH2:4][C:5]([CH3:7])=[O:6])=[O:3].[CH3:8][C:9]([CH2:11][C:12]([CH3:14])=[O:13])=[O:10].CC(CC(C)=O)=O.[Co:22].C1(C)C=CC=CC=1.C(NCCNCCCC)CCC>O>[CH3:7]/[C:5](/[OH:6])=[CH:4]\[C:2]([CH3:1])=[O:3].[CH3:14]/[C:12](/[OH:13])=[CH:11]/[C:9]([CH3:8])=[O:10].[Co:22]

참가 물질

5

반응물 3

HCID 1140TolueneHCID 77629N,N'-DibutylethylenediamineHCID 407384Cobalt(3+) acetylacetonate2회

생성물 1

HCID 5884498Cobalt (II) acetylacetonate

시약·촉매·용매 1

HCID 962Water용매

실험 절차

Several secondary diamine adducts of cobalt(II) acetylacetonate were prepared by adding 1.04 grams (4 millimoles) of cobalt acetylacetonate into a 50 ml two-necked flask. There was then added 30 ml of freshly distilled toluene along with a stir bar. The mixture was heated and residual water bound to the cobalt acetylacetonate was azotropically removed. When the distillation temperature reached 110° C., heating of the mixture was discontinued. There was then added 0.76 grams (4.4 millimoles) of N,N'-dibutylethylenediamine when the refluxing had subsided. The solution was stirred for one hour and allowed to cool. The product was crystallized from the solution after removal of some of the solvent by rotoevaporation. Recrystallization was effected from a hexane/methylenechloride mixture at -20° C. The same procedure was repeated except that in place of N,N'-di-t-butylethylenediamine there was added N,N'-t-N-butylethylenediamine. The following results were obtained:

후처리

  1. temperatureThe mixture was heated
  2. customwas azotropically removed
  3. customreached 110° C.
  4. temperatureheating of the mixture
  5. temperatureto cool
  6. customThe product was crystallized from the solution
  7. customafter removal of some of the solvent by rotoevaporation
  8. customRecrystallization
  9. customwas effected from a hexane/methylenechloride mixture at -20° C
  10. additionthere was added N,N'-t-N-butylethylenediamine
  11. customThe following results
  12. customwere obtained

출처 및 근거

ORD 기록
ord-e1c3be93d9ec40c2acbe671a8b0a5b0f
출처 데이터셋
uspto-grants-1989_08
특허 번호
US04855467

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