Methanamine, N-methyl-, titanium(4+) salt (4:1) → HCID 178423719, compound

HRID 15699Notes

Reaction equation

HRID 15699 reaction equation
[CH3:1][C:2]1[CH:3]([C:10]2[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=2[CH2:12][OH:13])[C:4]([CH3:9])=[C:5]([CH3:8])[C:6]=1[CH3:7].[CH3:18][N-:19][CH3:20].[CH3:21][N-:22][CH3:23].C[N-]C.C[N-]C.[Ti+4:30]>C1(C)C=CC=CC=1>[CH3:18][N-:19][CH3:20].[CH3:21][N-:22][CH3:23].[CH3:1][C:2]1[CH:3]([C:10]2[CH:17]=[CH:16][CH:15]=[CH:14][C:11]=2[CH2:12][O:13][Ti+2:30])[C:4]([CH3:9])=[C:5]([CH3:8])[C:6]=1[CH3:7]

Participants

4

Reactant 2

HCID 123185Methanamine, N-methyl-, titanium(4+) salt (4:1)HCID 1317271142-(2,3,4,5-Tetramethylcyclopentadienyl)benzylalcohol

Product 1

HCID 178423719HCID 178423719, compoundYield 83.3%

Reagents, catalysts & solvents 1

HCID 1140TolueneSolvent2×

Procedure

To a solution of 2-(2,3,4,5-tetramethylcyclopentadienyl)benzylalcohol (0.3 g, 1.3 mmol) in toluene (5.2 mL) was added dropwise a solution of tetrakis(dimethylamido)titanium (0.29 g, 1.3 mmol) in toluene (1.7 mL) at −30° C. The mixture was stirred for 30 min at room temperature and then at 110° C. for 5 hrs. The solvent was distilled off to give 2-(2,3,4,5-tetramethylcyclopentadienyl)benzyloxytitanium bis(dimethylamide) (0.30 g, yield 83.3%).

Workup

  1. waitat 110° C. for 5 hrs
  2. distillationThe solvent was distilled off

Sources & evidence

ORD record
ord-58329dbecfc44d7b8b368735b32723af
Source dataset
uspto-grants-2010_06
Patent number
US07732643B2

Reaction notes

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