Hexamethyltriethylene tetramine HMTETA

Caprolactone (CL) (Acros, 99%) was dried over calcium hydride at r.t. for 48h and then distilled under reduced pressure. 2-(N,N-dimethylamino)ethyl methaciylate (DMAEMA) (Aldrich, 98%) was deprived of its inhibitor by filtration through a basic alumina column, and depending on samples (see text) dried over calcium hydride at r.t. for 24h and then distilled under reduced pressme. Butane-1,4-diol (Acros, > 99%) was dried over calcium hydride for 48h at r.t. and distilled at 70°C under reduced pressure. Triethylamine (NEts, Fluka, 99%) was dried over barium oxide for 48h at r.t. and distilled under reduced pressure. Copper bromide (CuBr, Fluka, 98%) was purified in acetic acid and recrystallized in ethanol under inert atmosphere until a white powder is obtained. Tin(ll) bis-2-ethyl hexanoate (Sn(Oct)2, Aldrich, 95%), methacrylic anhydride (Aldrich, 94%), N,N-dimethylamino-4-pyridine (DMAP, Acros 99%), 1,1,4,7,10,10-hexamethyltriethylene tetramine (HMTETA, Aldrich, 97%), ethyl-2-bromoisobutyrate (E BBr, Aldrich, 98%), N,N-dicyclohexylcarbodiimide (DCC, Acros, 99%), were used as received. Tetrahydrofuran (THF, Labscan, 99%) was dried over molecular sieves (4A) and distilled over polystyryl lithium (PS LC) complex under reduced pressure just before use. Toluene (Labscan, 99%) was dried by refluxing over CaH2. 

Materials. The a,co-(3-hydroxypropyl)polydimethylsiloxane was a gift of Rhodia Silicones. All other chemicals were purchased from Aldrich, unless stated. 3,5-dinitrobenzoyl chloride (98%), 9H-carbazole-9-ethanol (95%), dichloromethane (for analysis), octamethylcyclotetrasiloxane (D, Shin-Etsu, 99%), TONSIL EXE0096 (Siid-Chemie), 2-bromoisobutyryl bromide (98%), HMTETA (1,1,4,7,10,10-hexamethyltriethylene tetramine, 98%), copper bromide (98%) and triethylamine (98%) were used as received. Methacryloyl chloride (97%) was distilled before use. All reactions were carried out under inert nitrogen atmosphere. 

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