N,N'-Diphenyl-P-Phenylenediamine → HCID 66643588, compound

Participants

Reaction Conditions

Reaction Steps

Into a 3-neck 250 mL round-bottomed flask were weighed, in the following order: 2-(2-phenylpropan-2-ylthio)ethanol (30.0 g, 0.1528 moles), N,N′-diphenyl-1,4-phenylene diamine (0.318 g, 1.2224×10−3 moles) and ethyl acrylate (122.40 g, 1.2224 moles). The apparatus was then assembled in a reactive distillation arrangement before being purged with N2 (g). The Claisen head of the distillation apparatus was wrapped with Al-foil/glass wool. The reaction flask was then heated to 120° C., by use of a silicone heating oil bath, and once the ethyl acrylate (Bpt: 99° C.) started to distil over tetrapropoxytitanate (TPT) (1.04 mL, 0.999 g, 3.5144×10−3 moles) was added to the reaction mixture via a 2.50 mL Hamilton gastight syringe. The distillation rate immediately increased significantly and the distillation vapour temperature decreased from 98° C. to ca. 80° C.

Provenance & Evidence