No. 179.
Deoxyanisoin
HARRY A. ROSE and JOHN G. WILLIAMS Eli Lilly and Co., Indianapolis 6, Ind. 0
il
H ~ C O -~ C H ~ - C - ~ - O C H ~ Structural Formula
D
can be crystallized from ethanol or benzene. I n both cases the resulting crystals are needles elongated parallel to the b axis, The crystals usually show the 001 and T O 1 faces and occasionally the 100. The x-ray powder diffraction data were obtained using a camera 114.6 mm. in diameter and copper radiation with nickel filter. A wave length value of 1.5405 A. was used in the calculations. The indexing was done on the basis of a single crystal rotation pattern and a Weissenberg pattern around the b axis. EOXYANISOIN
CRYSTAL MORPHOLOGY Crystal System. Monoclinic. Form and Habit. Seedles elongated parallel to b. Axial Ratio. a : b : c = 3.905:1:2.815. Beta Angle. 135" 52'. X-RAYDIFFRACTION D.4TA Cell Dimensions. % = 21.71 A., bo = 5.56A., Q = 15.65A.
1/11 hkl 0.13 OOL 0.13 202 0.05 002,402 110 0.05 0.08 011 0.05 201 1.00 210 0.67 111 0.13 012 0.67 400 0.26 202 0.20 410 0.40 405,605, 013
d 11.04 7.93
_ .
5.50 5.21 4.91 4.83 4.48 4.31 3.86 3.81 3.41 3.12 3.08
X-Ray Powder Diffraction Data d (Calcd.) d I/Il 10.90 7.83 5.45,5.43 5.22 4.95 4.80 4.48 4.31 3.89 3.80 3.41 3.13 3.07,3.06, 3.04
Formula TVeights per Cell. 4. Formula Weight. 256.30. Density. 1.287 grams per cc. (flotation), 1.296 grams per cc. (x-ray). OPTICALPROPERTIES Refractive Indices. CY = 1.524, p = 1.624, y > 1.70. ODtic Axial Angle. 2V = 85" (estfmated) . Optic Axial Plane. Perpendicular to 010.
-
2.92 2.73 2.59b 2.45 2.41 2.32 2.29 2.25 2.21 2.17 2.07 2.02
0.01 0.05 0.08 0.03 0.03 0.05 0.05 0.08 0.08 0.05 0.08 0.01
hkl 212 004 220,121 022
d (Calcd.) 2.91 2.73 2.61,2.59 2.45
Optic Sign. Positive. Extinction. CY A a = 8"in obtuse 0. Orientation. 6 = b. FESIOXBEHAVIOR. Deoxyanisoin melts in the range 110.0-11.5° C. as determined on a Kofler hot stage. KO polymorphism was observed. CRYSTdLLOGRAPHIC data for publication in this section should be sent to \Ti. C. McCrone, 501 East 32nd Rt., Chicago 16, Ill.
Composition of Methyl Methacrylate-Butadiene Copolymers R.
M. B.
CS-71
SMALL, Polymer Corp., Ltd., Sarnia, Ontario, Canada
Cell Windows: N a C l Absorbance Measuremenf:
I
No.1 1
Component Name Formula Poly-C4H602methyl methacrylate
-
Accuracy
Range
1
%
~
I
Calculation:
lduplicate
0.25on
1725 '0.005 cm-'2.1
MMA portion
cm-'
0.05
i1
- _ _ _ _ I
2
trans-l,4- -C Polybutadiene
I
cH 6-
5- 100 0.6 on butadiene
0.0115 0.15 on butacm-' 0.64
967
cm-'
e;.i:
diene
These d a t a represent standard publication and submission is open t o anyone in accordance with regulations of ANALYTICALCHEMISTRY. T h e Coblentz Society is acting only as a n aid t o the journal.
478
ANALYTICAL CHEMISTRY
Base line-
Inverse matrix& Graphical-
%
(0-100 10.2 ~
Instrument: Perkin-Eimer M o d e l 21, NaCl prism Sample Phase: Solution (1) dichloromethane; (2 and 31 carbon disulfide P o i n t 2 Successive approx.-
Relative Absorbancesa-Analytical Matrix: ComponentlX 1725 cm-' 1
2 3
4.31
(concn. w/w 967 cm-'
0.317 2.99 0.264
%,
length mm):
909 cm-' 0.124 0.035 3.87
Material Purify: Purified homopolymer, 99%; NBS trans-4-octene 99.8%; NBS 3-methyl-1 -pentene, 99.5%. Comments: M M A is industrial jargon for methyl methacrylate, both monomeric and polymeric. a Relative absorbances a r e given as the slope of the Beer's l a w concentration curves used expressed i n terms of absorbance per 100% of constituent.
T o standardize procedures ~ X C I L Y T I C A LCHEMISTRY requests t h a t material be sent in quintuplicate t o tdeAchairrnrtnof the review committee: Robert C. Wilkerson, Celanese Corp. of America, Post Office Box 8, Clarkwood, Tex.
