Details for Patent: 9,296,756

Title:	Crystal of 6,7-unsaturated-7-carbamoyl morphinan derivative and method for producing the same
Abstract:	Stable crystalline forms of a compound represented by the formula (IA): ##STR00001## an acid addition salt, and/or a solvate thereof are provided by the present invention. Said crystalline forms are extremely useful as materials for preparing medicines. Novel processes for preparing 6,7-unsaturated-7-carbamoyl morphinan derivatives are also provided by the present invention.
Inventor(s):	Inagaki; Masanao (Toyonaka, JP), Morimoto; Kenji (Toyonaka, JP), Haga; Nobuhiro (Toyonaka, JP), Oda; Shinichi (Iwate-ken, JP)
Assignee:	Shionogi & Co., Ltd. (Osaka, JP)
Filing Date:	Aug 04, 2015
Application Number:	14/818,152
Claims:	1. A process for preparing a compound of the formula (II): ##STR00049## wherein R.sup.1b is a hydroxy-protecting group, R.sup.2 is optionally substituted lower alkyl, and R.sup.3 is optionally substituted lower alkyl, optionally substituted cycloalkyl, optionally substituted aryl or optionally substituted heteroaryl, comprising: reacting a compound of the formula (III): ##STR00050## wherein R.sup.1b and R.sup.2 is the same as defined above, in the presence or absence of an acid with a compound of the formula: R.sup.3--N.dbd.C.dbd.O, wherein R.sup.3 is the same as defined above, or with a compound of the formula: R.sup.3--NH--C(.dbd.O)--X, wherein R.sup.3 is the same as defined above and X is a leaving group. 2. The process according to claim 1, wherein the compound of the formula (III) is obtained by protecting hydroxyl of a compound of the formula (IV): ##STR00051## wherein R.sup.2 is the same as defined in claim 1. 3. The process according to claim 2, wherein after the compound of the formula (III) is obtained from the compound of the formula (IV); the compound of the formula (III) is reacted successively with the compound of the formula: R.sup.3--N.dbd.C.dbd.O, or with the compound of the formula: R.sup.3--NH--C(.dbd.O)--X in the presence or absence of an acid. 4. The process according to claim 1, wherein the reaction of the compound of the formula (III) with the compound of the formula: R.sup.3--N.dbd.C.dbd.O or the compound of the formula R.sup.3--NH--C(.dbd.O)--X is carried out in the presence of an acid. 5. The process according to claim 4, wherein the acid is a Lewis acid. 6. The process according to claim 5, wherein the Lewis acid is CuCl, CuCl.sub.2, CuBr, CuI, CuBr, CuSO.sub.4, Cu, Zn(OAc).sub.2, ZnBr.sub.2 or ZnCl.sub.2. 7. The process according to claim 4, wherein the acid is present in an amount about 0.00005-1.0 molar equivalents to the compound of the formula (III). 8. The process according to claim 1, wherein R.sup.1b is a hydroxyl-protective group deprotectable by a base.