1-Methyl-1,3-cyclopentadiene → HCID 178484295、化合物

HRID 1613838ノート

反応式

HRID 1613838 の反応式
[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

参加物

4

反応物 2

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

生成物 1

HCID 178484295HCID 178484295、化合物

試薬・触媒・溶媒 1

HCID 1140Toluene溶媒

実験手順

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.

後処理

  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

出典と根拠

ORDレコード
ord-56cefdd766424a3db0d4394dde6d901b
出典データセット
uspto-grants-1993_03
特許番号
US05194532

反応ノート

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