Crystals of N-(trans-4-isopropylcyclohexycarbonyl)-D-phenylalanine and methods for preparing them
DCFirst Claim
1. A method for the production of crystals of N-(trans-4-isopropylcyclohexylcarbonyl)-D-phenylalanine having at least one of the following properties:
- (a) a melting point in the range of 136°
-142°
C.;
(b) a powder X-ray diffraction pattern with reflection maxima at 2θ
of about 8.1°
, 13.1°
, 19.6° and
19.9°
;
comprising dissolving or suspending N-(trans-4-isopropylcyclohexylcarbonyl)-D-phenylalanine in a solvent in which it is completely or incompletely soluble at a temperature of at least 10°
C. and up to the boiling point of the solvent and permitting said crystals to crystallize from or form in said solvent at a temperature of 10°
C. or in excess thereof.
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Abstract
Stable crystals of N-(trans-4-isopropylcyclohexylcarbonyl)-D-phenylalanine may be produced by treating this compound with a solvent at a temperature of at least 10° C. and forming crystals in the solvent at a temperature of at least 10° C. For example, crystals may be formed by crystallization out of solution, or may be formed from solid particles of the compound suspended in a solvent. Crystals formed in this way have different melting point, infra red spectrum and X-ray diffraction patterns from previously known forms of the compound and have enhanced processability, eg. stability to grinding.
46 Citations
13 Claims
-
1. A method for the production of crystals of N-(trans-4-isopropylcyclohexylcarbonyl)-D-phenylalanine having at least one of the following properties:
-
(a) a melting point in the range of 136°
-142°
C.;(b) a powder X-ray diffraction pattern with reflection maxima at 2θ
of about 8.1°
, 13.1°
, 19.6° and
19.9°
;
comprising dissolving or suspending N-(trans-4-isopropylcyclohexylcarbonyl)-D-phenylalanine in a solvent in which it is completely or incompletely soluble at a temperature of at least 10°
C. and up to the boiling point of the solvent and permitting said crystals to crystallize from or form in said solvent at a temperature of 10°
C. or in excess thereof. - View Dependent Claims (2, 3, 4, 5, 6, 7, 11)
-
-
8. Crystals of N-(trans-4-isopropylcyclohexylcarbonyl)-D-phenylalanine having at least one of the following properties:
-
(a) a melting point in the range of 136°
-142°
C.; and(b) a powder X-ray diffraction pattern with reflection maxima at 2θ
of about 8.1°
, 13.1°
, 19.6° and
19.9°
. - View Dependent Claims (9, 12)
-
- 10. Crystals of N-(trans-4-isopropylcyclohexylcarbonyl)-D-phenylalanine having an X-ray powder diffraction pattern as shown in FIG. 3.
Specification