1-Methyl-1,3-cyclopentadiene → HCID 178484295, 화합물

HRID 1613838노트

반응식

HRID 1613838 반응식
[CH3:1][N-:2][CH3:3].[CH3:4][N-:5][CH3:6].[CH3:7][N-:8][CH3:9].[CH3:10][N-]C.[Ti+4:13].C[C:15]1[CH2:19][CH:18]=[CH:17][CH:16]=1>C1(C)C=CC=CC=1>[CH3:1][N-:2][CH3:3].[CH3:4][N-:5][CH3:6].[CH3:7][N-:8][CH3:9].[CH3:10][Ti+3:13][CH:18]1[CH:17]=[CH:16][CH:15]=[CH:19]1

참가 물질

4

반응물 2

HCID 667751-Methyl-1,3-cyclopentadieneHCID 123185Methanamine, N-methyl-, titanium(4+) salt (4:1)

생성물 1

HCID 178484295HCID 178484295, 화합물

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A 250 mL Schlenk flask is charged with titanium tetrakis(dimethylamide), 3.73 g (16.64 mmole), and toluene, 100 mL. Methylcyclopentadiene, 5.33 g (66.54 mmole), is added to the magnetically stirred solution. The mixture is refluxed 1.5 hours. Solvent and volatiles are removed under vacuum leaving a brown residue. The residue is transferred to a microdistillation apparatus and a forerun of titanium tetrakis(dimethylamide) is distilled from the mixture (at 35°-40° C. and 0.025 mm Hg) followed by a red low melting solid (at 104°-108° C. and 0.025 mm Hg) which is determined to be methylcyclopentadienyltitanium tris(dimethylamide) by proton NMR.

후처리

  1. temperatureThe mixture is refluxed 1.5 hours
  2. customSolvent and volatiles are removed under vacuum
  3. customleaving a brown residue
  4. distillationa forerun of titanium tetrakis(dimethylamide) is distilled from the mixture (at 35°-40° C. and 0.025 mm Hg)
  5. customfollowed by a red low melting solid (at 104°-108° C. and 0.025 mm Hg) which

출처 및 근거

ORD 기록
ord-56cefdd766424a3db0d4394dde6d901b
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05194532

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