Zirconium, tetrakis(dimethylamino)- → HCID 178445890, 화합물

HRID 441779

반응식

HRID 441779 반응식
[CH2:1]([Li])[C:2]([CH3:5])([CH3:4])[CH3:3].[CH3:7][N-:8][CH3:9].[CH3:10][N-:11][CH3:12].[CH3:13][N-:14][CH3:15].C[N-]C.[Zr+4:19]>CCCCCC.CCCCC>[CH3:7][N-:8][CH3:9].[CH3:10][N-:11][CH3:12].[CH3:13][N-:14][CH3:15].[CH2:1]([Zr+3:19])[C:2]([CH3:5])([CH3:4])[CH3:3]

참가 물질

5

반응물 2

HCID 140580Zirconium, tetrakis(dimethylamino)-HCID 178506860HCID 178506860, 화합물

생성물 1

HCID 178445890HCID 178445890, 화합물

시약·촉매·용매 2

HCID 8003Pentane용매HCID 8058Hexane용매2회

실험 절차

A solution of 0.50 g of neopentyllithium in hexane was added to a hot solution of zirconium tetrakis(dimethylamide) in hot hexane with stirring. Lithium dimethylamide precipitated immediately. The total amount of hexane in the reaction mixture was about 50-100 ml. The mixture was cooled and filtered, and the filtrate was evaporated to give a sticky solid. The latter was dissolved in pentane, and the solution was kept at -40° C. for 2 days. During this time yellow crystals of neopentylzirconium tris(dimethylamide) separated. They were isolated by filtration and dried; yield 0.5 g. Nmr in C6D6 : δ (NMe) 2.92, δ (CH2) 0.9, δ (CMe3) 1.20 ppm downfield from tetramethylsilane.

후처리

  1. customLithium dimethylamide precipitated immediately
  2. temperatureThe mixture was cooled
  3. filtrationfiltered
  4. customthe filtrate was evaporated
  5. customto give a sticky solid
  6. customDuring this time yellow crystals of neopentylzirconium tris(dimethylamide) separated
  7. customThey were isolated by filtration
  8. customdried

출처 및 근거

ORD 기록
ord-cd571245a2694fb0bcdbee6337ed4849
출처 데이터셋
uspto-grants-1977_08
특허 번호
US04042610

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