ANALYTICAL CHEMISTRY
1790 LITERATZTRE CITED
(1) Duteher, J. D., Donin, M. N., J. Am. Chem. SOC.74, 3420-2 (1952). (2) Dutcher, J. D., Hosansky, N., Donin, M. N., Wintersteiner, 0.. Ibid., 73, 1384-5 (1951). (3) Duteher, J. D., Hosansky, N., Sherman, J. H., Antibiotics & Chemotherapy 3, 534-6 (1953). (4) Ford. J. H., Berm, & E., 'I Brooks, . A. A., Garrett. E. R., Alberti, J.. Dyer, J. R., Carter, H. E., J . Am. Cham. Soc. 77, 5311-14 (1955). (5) Hsmre, D. M., Pansy. F. E., Lepedes, D. N., Pedman, 0..
Bayan.A. P., Donoviek. R.. AnAbiotics & Chemotheram2, 13541 (1952). (6) Leach, B. E., Teeters, C. M., 3. Am. Chhem. Soc. 73, 2794-7 (1951). (7) O'Keefe, A. E.. Russo-Alesi. F. M., Division of Biological Chemistry, 116th Meeting, ACS, Atlantic City, N. J.. 1949. ( 8 ) Pan, S. C.. Dutcher, J. D., ANALCHEM. 28,836 (1956). (9) Sokolski, W. T.. Carpenter, 0. S., "Antibiotics Annual 19551956, P.383, Medical Encyelopedia. Ino., New York, 1956. (10) U. S. Pharmacopoeia, 15th Revision, p. 855, Mack Publishing Co., Easton, Pa.. 1956. R ~ c ~ ~ for v areview n ~ p r i 25, l 1956. Accepted jUly 20, 1956
CRYSTALLOGRAPHIC DATA
139. 2-Amino-2-methyl-l,3-propanediol HARRY A. ROSE end ANN VAN CAMP, Lilly Research Lsborstorior, Indianapolis 6, Ind.
HO-CHS
I I
CHa-C-NHs HO-CHs Structural formula for 2-amino-2-metYJ.-.,.-=~"~~"="~".
C
# =93O32' L a
2-h~1~o-Z-methyl-1,3-propsnediolcan be crystallized from acetone or from the lower alcohols. The crystals used in this study were obtained by allowing a warm isopropyl alcohol solution to cool. The resulting crystals are needles and rods elongated parallel to the c axis.
b-
L U M E 28, N O . 11, N O V E M B E R 1 9 5 6
1791
AY DIFFRACTION DATA
,I1Dimensions.
aa
= 8.62 A,, bo = 11.00 A,, co = 6.10
A.
irmula Weights per Cell. 4. Formula Weight. 105.14. Density. 1.211 grams per cc. (displacement), 1.211 grams per cc. (x-ray).
slowly without agitation over a period of several hours. Typical orystsls prepared in this manner are shown in Figures I and 2. The positions of the lead atoms in each of the polymorphic farms have been determined by Azaroff (1). Crystsk of Form I1 transform readily t o Form I in solution (Figure 3).
OPTICALPROPERTIES Refractive Indices (5893 A,, 25"C.), a
= 1.516, p = 1.528, 1.538. Optic Axial Angle. 2V = ( - ) 84"24' (calculated from a, 0,
y =
9"d " ) , _-_
O& Axial Plane. Perpendicular to 010 Acute Biseotrix. a. Extinction. a A e = 16" in itcute 8.
X-Ray Powder Diffraction Data d 6.81 5.33 5.12 4.83 4.65 4.30 4.08 3.75 3.43 3.37 3.26 3.14 2.98 2.90 2.73 2.66 2.57 2.46 2.41 2.39 2.35 2.23 2.04 1.990 1.905 1.850 1.795
hkl 110
1/Il 0.50 0.80 0.50 0.80 1.00
OIL
101 101 iii. 120
0.40 1.00 0.20 0.20 0.20
200 021
0.40 0.20 0.20 0.30 0.10 0.10
211 03_1
0.10b 0.20 0.10 0.10
12i
211 220
131 221 112
.
3oi . 23i.202 311 20! 141
d (Calod.! 6.78 5.33 5.12 4.83 4.64.4.6)
4.30 4.08 3.75 3.44 3.39 3.26 3.14 2.98 2.90 2.73 2.66 2.58.2.56 2.47 2.42 2.43
0.05 0.05
melt does not crystallize on cooling.
I
P r i n c i d Lines d 5.37 5.01 4.84 4.64 4.44
1/11
4.27
6
4.13 3.90 3.78 3.29
8
3.20 3.15 3.08 3.02 2.95
a
5
4 10 4
