Stoppers cyclohexyl

The [2]rotaxanes, which contain tetrathiafulvalene (TTF) and 1,5-dioxynaphtha-lene (DNP) as the two recognition stations and cyclobis(paraquat-p-phenylene) (CBPQT4 + ) as the cyclic moiety, have been comprehensively investigated by Stoddart and coworkers.68 We have recently reported two new TTF-DNP-CBPQT4+ [2]rotaxanes 62 and 63. In these two [2]rotaxanes, the TTF moiety is the 4,4 (5 )-dialkylthiotetrathiafulvalene that is rather easily accessible based on the synthetic procedure developed by us previously,69 and two different spacers are used the cyclohexyl and alkyl chains. Two stopper units are the G2-dendritic moieties. 

In a 100 ml flask fitted with a mechanical stirrer, a vertical condensor protected by a calcium chloride stopper, a dropping-funnel and a source of nitrogen were introduced 30 ml of hexamethylenephosphotriamide and 2.3 g (0.1 mol) of finely cut sodium wire. A mixture of 12.3 g (0.1 mol) of (3-thienyl)-acetonitrile and 16.3 g (0.1 mol) of cyclohexyl bromide was then quickly added at a temperature of 20 C. The reaction mixture was then maintained under nitrogen atmosphere and stirred for 12 hours at room temperature. The excess of sodium was destroyed by adding 5 ml of ethanol and the organic solution was slowly poured into 100 ml of a 1 N iced solution of hydrochloric acid. The solution was extracted twice with 100 ml ether. The ethereal phases were collected, washed with water, dried and concentrated under reduced pressure. The crude product was then purified by... 

Etofenprox calibration solution. Weigh in duplicate (to the nearest 0.1 mg) about 0.06 g of etofenprox standard (M and Mg) into two 50-ml stoppered volumetric flasks. Add 10ml of di-cyclohexyl phthalate internal standard solution, shake to dissolve the etofenprox and dilute to 50 ml with methanol/tetrahydrofuran (50 50, v/v) (solutions and Cg). Keep the solutions in a thermostat bath if room temperature varies by more than 2°C. 

B) Hydrolysis of Monohalides. (1) The following halides are used in this test n-butyl chloride, ec-butyl chloride, tert-butyl chloride, n-amyl chloride, cyclohexyl chloride, phenyl chloride chlorobenzene), and benzyl chloride. For the student s use the pure halides are placed in 25 ml bottles provided with droppers which serve also as stoppers to the bottle. The dropper is replaced in the bottle immediately after use. 

Cyclohexanol in ether added with stirring at 0° to o-phenylene phosphorochloridite (prepn. s. Synth. Meth. 14, 159) and pyridine in ether, stoppered, allowed to warm to 25°, and the product isolated after 12 hrs. cyclohexyl o-phenylene phosphite (Y 95.4%) dissolved in methylene diloride, treated with iodine, stirred 6 hrs. at 25°, and extracted successively with 5%-NaOH-soln., NaHSOg-soln., and satd. NaCl-soln. -> cyclohexyl iodide (Y 87.4%). Overall Y 83.2%. F. e. s. E. J. Corey and J. E. Anderson, J. Org. Chem. 32, 4160 (1967). 

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