Hexamethylphosphoramide → HCID 131710512, compound

HRID 1729593Notes

Reaction equation

[Cl-:1].[Cl-].[Cl-].[Ti+3:4].[CH3:5][N:6]([CH3:15])[P:7](=[O:14])([N:11]([CH3:13])[CH3:12])[N:8]([CH3:10])[CH3:9]>>[CH3:5][N:6]([CH3:15])[P:7](=[O:14])([N:8]([CH3:10])[CH3:9])[N:11]([CH3:12])[CH3:13].[Cl-:1].[Cl-:1].[Cl-:1].[Ti+3:4]

Participants

Reactant 2

HCID 12679Hexamethylphosphoramide

HCID 10313229titanium(III) trichloride

Product 1

HCID 131710512HCID 131710512, compound

Procedure

133 gms of the titanium trichloride were introduced into a stainless steel ball mill, 9 inches long and 5.1 inches diameter containing 685 stainless steel balls of diameter 0.5 inches. Hexamethylphosphoric triamide (HMPT) was added as a solid in an amount calculated to give a molecular ratio HMPT/titanium trichloride of 0.167. The contents of the mill were shaken manually to disperse the HMPT over the particles of TAC 131 and the mill was rotated for 22 hours at 45 rpm. A nitrogen atmosphere was maintained in the mill at all times.

Sources & evidence

ORD record: ord-bf76f808f5354f56a3f4ec342e1be8df
Source dataset: uspto-grants-1976_11
DOI: 10.6084/m9.figshare.5104873.v1
Patent number: US03989641

Reaction notes

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