Oxidation of Cyclohexane with Cobalt (III) Vacuum Pyrolyses.-Samples (0.1 mmol) weighed into Pyrex boats were placed in a horizontal Pyrex pyrolysis tube whose entrance was then sealed off and whose exit led to a U-tube and thence to a vacuum line, the unit being formed from a single piece of glass. The system was pumped out to 10~3 Torr, the U-tube immersed in liquid N2, and the pyrolysis tube heated in an air bath at 250°for 1 hr followed by 30-45 min at 270-280°. The U-tube trap was then sealed off, removed, warmed to 0°, and opened.Reaction of AgNOg-RiNNOg with Carbon Tetrachloride.-Silver nitrate and tetrapentylammonium nitrate were weighed into a 5-ml ampoule and the mixture was protected from atmospheric moisture and heated at 100-110°for 24 hr to produce a homogeneous melt. CCh and any other additives were added to the cooled mixture via a microliter syringe, and the ampoule was sealed, heated under the conditions specified in the tables, chilled, and opened.Identification of dipentylnitrosamine in a typical product was accomplished by triturating with ether and filtering off AgCl, AgNOg, and RgNNOg. Evaporation of the filtrate left a yellow oil whose gc retention time, nmr and mass spectra were those of authentic dipentylnitrosamine. The ir spectrum was that of dipentylnitrosamine plus bands at 3500-2200, 1720, and 945 cm-1 attributable to valeric acid. Gas chromatographic evidence for both valeraldehyde and valeric acid was obtained but irreproducibility prevented quantitation.Pyrolysis of Tripentylammonium Nitrate.-A solution of 1.001 g (4.41 mmol) of tripentylamine in 40 ml of ethanol was treated

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ribo -4-(Benzylamino)hept-1 -ene-5, 6-diol (21). A resealable Carius tube was charged with 490 mg (3.83 mmol) of (+)-18, 0.42 mL (3.85 mmol) of benzylamine, 32 mg (0.34 mmol) of phenol, and 0.9 mg (0.04 mmol) of BHT. The tube was purged with argon and heated to 145 °C for 86 h. The crude product was dissolved in CH2C12 and concentrated in vacuo to give 971 mg of crude product. Recrystallization of this sample from Et^O-CCh afforded 366 mg (mp 62-64 °C) of pure 21 as bulky plates. The mother liquors were chromatographed on 90 g of silica gel (4% MeOH in CH2C12) to afford an additional 448 mg (814 mg total, 91% yield) of crystalline 21: [a]20D +27°(c 1.2, EtOH); NMR (CDCI3) 5 7.3 (s, 5 H, aromatic), 5.76 (m, 1 , H2), 5.13 (m, 2 H,

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