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Cholestan-3/3-ol-22-one (XXXVII) (A. Ercoli), R.D. (Fig. 4) in methanol (c 0.090): [o+oo -20°, [a]ss9-14°[ a]sic -305°, [a]27o +400°; acid study (40 min.), [a]700 + 5°, [a]sag +2°, [a]3io -180°, [a]302.6 +87°: at 310 µ, 35min. = -180°. (XXXVIII) (A. Ercoli), R.D. in methanol (c 0.121): [a]700 + 10°, [a]539 +10°, [a]310 -317°, [«jone +870°, [a]262.5 +830°; acid study (20 min.), [«]312 5 -294°: at 310 µ, 3 min. = -301°, 10 min. = -227°, 15 min. = -231°. 3-Methyl-3-phenylhexan-4-one (XXXIX) (D. J. Cram),39 R.D. in methanol (c 0.14): [a]700 +56°, [a+ss + 61°, [a]su +1588°, [a]307.5 +1176°; acid study (98 min.), [a] 700 +46°, [a] 589 +57°, [a]ai5 +1349°, [a]3io +1278°: at 315 µ, 94 min. = +1349°. 3,4,6-Trimethyl-5-oxoheptanoic acid (XL) (R. H. Eastman),40 R.D. in methanol (c 0.110): [a]700 +36°, [a]539 + 43°, [q]3!5 +914°, [a]300 +393°; acid study (20 min.), [a]700 +30°, [a]589 +40°, [a]3i5 +930°, [ajsio +836°: at 315 m^, 17 min. = +930°.Acknowledgment.-We are greatly indebted to the various authors listed in the Experimental section for gifts of samples. Detroit, Mich.

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t ‐Butyl azidoformate product: t ‐Butyl azidoformate

t ‐Butyl carbazate solvent: 430 ml. (422 g., 5.33 moles) of pyridine reactant: 508 ml. (395 g., 5.33 moles) of t ‐butyl alcohol reactant: 536 g. (4.85 moles) of methyl chlorothiolformate intermediate: 500 g. (3.47 moles) of t ‐butyl S‐methylthiolcarbonate solvent: 50‐50 mixture of low‐ (b.p. 30–60°) and high‐boiling (b.p. 60–70°) ligroin reactant: 430 g. (3.33 moles) of quinoline reactant: 520 g. (3.32 moles) of phenyl chloroformate intermediate: 388.4 g. (2.0 moles) of phenyl t ‐butyl carbonate solvent: petroleum ether product: t ‐Butyl carbazate product: bibenzyl