1966
J.Org. Chern., Vol. 40, No. 13, 1975
Weinshenker, Crosby, and Worig
temperature was k e p t a t -30'. Again n o optical r o t a t i o n was observed. C. T o a solution o f 48 (4.651 mg, 12.5 X lob3 m m o l ) in chlorom m o l ) in f o r m (10 m l ) was added ( + ) - T A P A (3.578 mg, 8 x c h l o r o f o r m (2 ml). T h e resulting solution was refluxed f o r 5 min a n d half o f t h e chloroform (6 m l ) was removed by distillation. A f t e r cooling a n d standing f o r 48 hr, t h e precipitated complex (0.988 mg) was separated f r o m t h e solution by decantation a n d washed w i t h 1 ml of cold chloroform. T h e solid was d r i e d a n d t h e n dissolved in 4 ml o f chloroform a n d t h e r o t a t i o n was measured. T h e observed values were a436 0.025', a546 0.005', a n d a578
