Ir film

Gas chromatographic analysis of the product on a 1-m column packed with 20% Silicone SE-30 at 180°C should give a single peak. The product has the fallowing spectral properties IR (film) cm" 1710, 1630 (C=C) ... 

Thermography The use of a tube or IR film to determine surface temperatures... 

Reaction of S-b-MM with Lithium Iodide. The reaction was carried out under nitrogen in a 250-mL, round-bottom flask equipped with a magnetic stirrer and a reflux condenser. To a solution of S-b-MM-90/10-wt (3.00 g, 3.0 meq MM) in toluene (100 mL) was added Lil (0.45 g, 3.4 mmol), and the mixture was refluxed for 20 hr. The solvent was partially evaporated, and the polymer was then precipitated from methanol. The precipitate was washed with methanol, water, and again with methanol. The dried polymer was reprecipitated, washed, and dried as described above, yielding 2.58 g of product. Analysis by 1H NMR shows only a trace of MM signal at 3.59 ppm IR (film) y 1723 and 1570 cm-1 (shoulder) ICP 0.106, 0.110 wt% Li (0.156 meq Li/g) expect 1.07 meq Li/g. 

A 2.09 g portion of this product was dissolved in THF (50 mL) and treated with cone. HC1 (3.33 mL, 40 meq) in water (5 mL). The mixture was refluxed for 4 hr. It was cooled, filtered to remove insoluble residue, and precipitated from 1 1 water-methanol. The precipitate was resuspended in dichloromethane, reprecipitated from methanol, washed, and dried as before, yielding 1.27 g IR (film) v 1732, 1701, 1199, and 1083 cm"1. 

A 0.42 g portion of the initial product from the reaction of MM-b-tBM with TMSI was converted to its potassium salt in the same manner as that previously described above for S-b-MA, yielding 0.20 g of MM-b-MA.K. Analyses IR (film) v 1729 and 1552 cm-1 ICP ... 

If desired, the product can be purified by column chromatograpy on 230-400 mesh silica gel (50 times by weight, elution with 5-10% ethyl acetate-hexane). (Tributylstannyl)methanol exhibits the following spectral properties IR (film) cm 1 3320, 2970, 2940, 2880, 2860, 1465, 1440, 1380, 1360, 1345, 1295, 1255, 1185,... 

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