阅读说明：本技术 6-(2,4-二氯苯基)-5-[4-[(3s)-1-(3-氟丙基)吡咯烷-3-基]氧基苯基]-8,9-二氢-7h-苯并[7]轮烯-2-甲酸甲酯的盐及其制备方法 (Salt of methyl 6- (2, 4-dichlorophenyl) -5- [4- [ (3S) -1- (3-fluoropropyl) pyrrolidin-3-yl ] oxyphenyl ] -8, 9-dihydro-7H-benzo [7] annulene-2-carboxylate and process for preparing same ) 是由 J·马拉蒂克 J·鲁伊斯·蒙特斯 于 2019-09-06 设计创作，主要内容包括：本文提供了6-(2,4-二氯苯基)-5-[4-[(3S)-1-(3-氟丙基)吡咯烷-3-基]氧基苯基]-8,9-二氢-7H-苯并[7]轮烯-2-甲酸甲酯的新型盐,即草酸盐(I)和二苯甲酰基酒石酸盐(II)。(Provided herein are 6- (2, 4-dichlorophenyl) -5- [4- [ (3S) -1- (3-fluoropropyl) pyrrolidin-3-yl]Oxy-phenyl]-8, 9-dihydro-7H-benzo [7]]Novel salts of methyl rotalene-2-carboxylate, namely oxalate (I) and dibenzoyltartrate (II).)

1. An oxalate salt of methyl 6- (2, 4-dichlorophenyl) -5- {4- [1- (3-fluoro-propyl) -pyrrolidin-3-yloxy ] -phenyl } -8, 9-dihydro-7H-benzocycloheptene 2-carboxylate of the formula:

2. a dibenzoyl tartrate salt of methyl 6- (2, 4-dichlorophenyl) -5- {4- [1- (3-fluoro-propyl) -pyrrolidin-3-yloxy ] -phenyl } -8, 9-dihydro-7H-benzocycloheptene 2-carboxylate of the formula:

3. a process for preparing the salt of claim 1, comprising the steps of:

oxalic acid is added to a compound (2) of the following formula in a solvent,

the solvent is selected from ester solvents, ether solvents and toluene.

4. The process according to claim 3, wherein the ester solvent is an acetate ester solvent, in particular ethyl acetate or isopropyl acetate.

5. The process according to claim 3, wherein the ethereal solvent is selected from the group consisting of methyl tert-butyl ether and diisopropyl ether.

6. The process according to any one of claims 3 or 4, wherein the ester solvent is isopropyl acetate.

7. The process according to claim 6, wherein the process is carried out in isopropyl acetate, under heating, in particular between 60 ℃ and 80 ℃ and more in particular at 70 ℃.

8. A process for preparing the salt of claim 2, comprising the steps of:

adding dibenzoyltartaric acid to a compound (2) of the formula in a mixture of toluene and heptane