Indene → HCID 178484298, 화합물

HRID 1613831노트

반응식

HRID 1613831 반응식
[CH3:1][N-:2][CH3:3].[CH3:4][N-:5][CH3:6].[CH3:7][N-:8][CH3:9].C[N-]C.[Ti+4:13].[CH2:14]1[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH:16]=[CH:15]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].[CH:14]1([Ti+3:13])[C:22]2[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=2)[CH:16]=[CH:15]1

참가 물질

4

반응물 2

HCID 7219IndeneHCID 123185Methanamine, N-methyl-, titanium(4+) salt (4:1)

생성물 1

HCID 178484298HCID 178484298, 화합물수율 70%

시약·촉매·용매 1

HCID 1140Toluene용매

실험 절차

A 250 mL Schlenk flask is charged with toluene, 75 mL, and titanium tetrakis(dimethylamide), 2.35 g (10.48 mmole). The mixture is stirred magnetically throughout the procedure. Freshly degassed indene (nitrogen sparged) is added to the Schlenk flask at room temperature in excess, 2.44 mL (20.96 mmole). The mixture is refluxed at least 24 hours giving a blood red solution. All volatiles are removed under vacuum at room temperature leaving a deep red, oily residue. The residue is transferred in a minimum of hexane to a micro scale distillation apparatus and distilled under vacuum. A viscous red oil distills at 60° C. (0.025 mm Hg) which is identified by nuclear magnetic resonance (NMR) as indenyltitanium tris(dimethylamide). The yield is 70% by this method of preparation.

후처리

  1. temperatureThe mixture is refluxed at least 24 hours
  2. customgiving a blood red solution
  3. customAll volatiles are removed under vacuum at room temperature
  4. customleaving a deep red, oily residue
  5. distillationThe residue is transferred in a minimum of hexane to a micro scale distillation apparatus
  6. distillationdistilled under vacuum
  7. distillationA viscous red oil distills at 60° C. (0.025 mm Hg) which
  8. customThe yield is 70% by this method of preparation

출처 및 근거

ORD 기록
ord-8bea02ef4d0c48528faa8b914048ff06
출처 데이터셋
uspto-grants-1993_03
특허 번호
US05194532

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