Methanamine, N-methyl-, titanium(4+) salt (4:1) → HCID 178484297, compound

HRID 441778Notes

Reaction equation

HRID 441778 reaction equation
[CH3:1][N-:2][CH3:3].[CH3:4][N-:5][CH3:6].[CH3:7][N-:8][CH3:9].C[N-]C.[Ti+4:13].[CH3:14][Si:15]([CH2:18][Li])([CH3:17])[CH3:16]>CCCCC>[CH3:1][N-:2][CH3:3].[CH3:4][N-:5][CH3:6].[CH3:7][N-:8][CH3:9].[CH3:14][Si:15]([CH2:18][Ti+3:13])([CH3:17])[CH3:16]

Participants

4

Reactant 2

HCID 123185Methanamine, N-methyl-, titanium(4+) salt (4:1)HCID 178418939HCID 178418939, compound

Product 1

HCID 178484297HCID 178484297, compoundYield 17.4%

Reagents, catalysts & solvents 1

HCID 8003PentaneSolvent2×

Procedure

To a stirred solution of 4.20 g of titanium tetrakis(dimethylamide) in about 10 ml of pentane was added a solution of 1.77 g of trimethylsilylmethyllithium in pentane. Lithium dimethylamide precipitated immediately. The mixture was stirred for 1 hour and filtered, pentane was removed from the filtrate by rotary evaporation, and the residual pale-yellow oil was distilled through a short still-head under reduced pressure, to give 0.87 g of trimethylsilylmethyltitanium tris(dimethylamide), bp 55° C. (50 μ). Nmr in C6D6 : δ (NMe) 3.07, δ (SiMe) 0.22, δ (CH2) 0.35 ppm downfield from tetramethylsilane.

Workup

  1. customLithium dimethylamide precipitated immediately
  2. filtrationfiltered
  3. custompentane was removed from the filtrate by rotary evaporation
  4. distillationthe residual pale-yellow oil was distilled through a short still-head under reduced pressure

Sources & evidence

ORD record
ord-4b264f5fd10243c9b7cc9fc8b72f0a0e
Source dataset
uspto-grants-1977_08
Patent number
US04042610

Reaction notes

Loading…