Toluene → HCID 178478906, compound

HRID 564963Notes

Reaction equation

HRID 564963 reaction equation
[Ti](Cl)(Cl)(Cl)[Cl:2].C1(C)C=CC=CC=1.[Cl-:13].[C:14]1([N:20]2[CH2:28][CH2:27][N:26]([Ti+3:29])[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)[CH:19]=[CH:18][CH:17]=[CH:16][CH:15]=1.[Cl-].[Cl-]>C(OCC)C>[Cl-:2].[Cl-:13].[C:14]1([N:20]2[CH2:28][CH2:27][N:26]([Ti+2:29])[CH2:25][CH2:24][NH:23][CH2:22][CH2:21]2)[CH:15]=[CH:16][CH:17]=[CH:18][CH:19]=1

Participants

5

Reactant 3

HCID 1140TolueneHCID 24193Titanium TetrachlorideHCID 178478624HCID 178478624, compound

Product 1

HCID 178478906HCID 178478906, compound

Reagents, catalysts & solvents 1

HCID 3283Diethyl EtherSolvent

Conditions

Temperature
40 °C

Procedure

Separately, 0.647 g (3.41 millimoles) of titanium tetrachloride was dissolved in 20 milliliters of diethyl ether at −50° C. The resulting solution was dropwise added at −60° C. over 2 hours to the toluene mixed solution prepared previously, and the resulting mixture was then heated to 40° C. and then subjected to reaction for a further 6 hours. Subsequently, the reaction mixture obtained was subjected to recrystallization from a hexane/methylene chloride mixed solvent to isolate the product, thereby obtaining N-phenyl-1,4,7-triazacyclononanyltitanium chloride in a yield of 35%.

Workup

  1. customprepared previously
  2. customsubjected to reaction for a further 6 hours
  3. customSubsequently, the reaction mixture obtained
  4. customwas subjected to recrystallization from a hexane/methylene chloride mixed solvent
  5. customto isolate the product

Sources & evidence

ORD record
ord-0e054174e4324173818f9deff4cf1365
Source dataset
uspto-grants-2001_01
Patent number
US06169152A

Reaction notes

Loading…