Optically active pyranochromenyl phenol derivative and pharmaceutical composition comprising same
a technology of pyranochromenyl phenol and phenol derivative, which is applied in the direction of drug composition, organic racemisation, metabolic disorder, etc., can solve the problems of difficult to develop a product actually utilizing glabridin, rapid increase in obesity ratio, etc., and achieve excellent anti-obesity efficacy, excellent anti-diabetic effect, and chemical stability. high
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example 1
Preparation of (R)-3-(2-hydroxy-4-ethoxyphenyl)-8,8-dimethyl-2,3,4,8,9,10-hexahydropyrano[2,3-f]chromene (Compound 1a) and (S)-3-(2-hydroxy-4-ethoxyphenyl)-8,8-dimethyl-2,3,4,8,9,10-hexahydropyrano[2,3-f]chromene (Compound 1b)
[0096]3-(2-hydroxy-4-ethoxyphenyl)-8,8-dimethyl-2,3,4,8,9,10-hexahydropyrano[2,3-f]chromene in the form of a racemic compound was synthesized in accordance with the method exemplified in Korean Patent Application Laid-Open No. 10-2015-0075030 (Patent Document 2).
1-1: Preparation of 2-(2-benzyloxy-4-ethoxyphenyl)-3-(2,2-dimethyl-5-hydroxy-2H-1-benzopyran-6-yl)-acrylic acid methyl ester
[0097]A three-neck round flask was cooled in a dry ice-acetone bath at −78° C. while being maintained under a nitrogen atmosphere, and 45 ml of a 1.0 M lithium diisopropyl amide (LDA)-THF solution was added thereto. Thereafter, 8.10 g (30.0 mmol) of (2-benzyloxy-4-ethoxyphenyl)acetic acid methyl ester was dissolved in 150 ml of THF, and then the resulting solution was slowly added ...
example 2
Preparation of (R)-3-(2-hydroxy-4-propoxyphenyl)-8,8-dimethyl-2,3,4,8,9,10-hexahydropyrano[2,3-f]chromene (Compound 2a) and (S)-3-(2-hydroxy-4-propoxyphenyl)-8,8-dimethyl-2,3,4,8,9,10-hexahydropyrano[2,3-f]chromene (Compound 2b)
[0115]3-(2-hydroxy-4-propoxyphenyl)-8,8-dimethyl-2,3,4,8,9,10-hexahydropyrano[2,3-f]chromene was synthesized in the form of a racemic compound by using the same method as in Example 1, except that in Example 1-1, (2-benzyloxy-4-propoxyphenyl) acetic acid methyl ester was used instead of (2-benzyloxy-4-ethoxyphenyl) acetic acid methyl ester. Daicel Chiral Technologies Co., Ltd. was requested for the separation and purification of the synthesized sample, 10 g of an R-enantiomer and 10 g of an S-enantiomer with >99% ee were provided, and the results of 1H-NMR, 13C-NMR, optical rotation, and M.P. for the enantiomers are shown as follows.
[0116]1H-NMR (CDCl3): 6.976 (d, 1H, J=8.4 Hz), 6.817 (d, 1H, J=8.0 Hz), 6.452 (dd, 1H, J=8.0, 2.0 Hz), 6.392 (d, 1H, J=8.4 Hz), ...
example 3
Preparation of (R)-3-(2-hydroxy-4-butoxyphenyl)-8,8-dimethyl-2,3,4,8,9,10-hexahydropyrano[2,3-f]chromene (Compound 4a) and (S)-3-(2-hydroxy-4-butoxyphenyl)-8,8-dimethyl-2,3,4,8,9,10-hexahydropyrano[2,3-f]chromene (Compound 4b)
[0124]3-(2-hydroxy-4-butoxyphenyl)-8,8-dimethyl-2,3,4,8,9,10-hexahydropyrano[2,3-f]chromene was synthesized in the form of a racemic compound by using the same method as in Example 1, except that in Example 1-1, (2-benzyloxy-4-butoxyphenyl) acetic acid methyl ester was used instead of (2-benzyloxy-4-ethoxyphenyl) acetic acid methyl ester. Daicel Chiral Technologies Co., Ltd. was requested for the separation and purification of the synthesized sample, 10 g of an R-enantiomer and 10 g of an S-enantiomer with >99% ee were provided, and the results of 1H-NMR, 13C-NMR, optical rotation, and M.P. for the enantiomers are shown as follows.
[0125]1H-NMR (CDCl3): 7.009 (d, 1H, J=8.4 Hz), 6.847 (d, 1H, J=8.0 Hz), 6.482 (dd, 1H, J=8.0, 2.0 Hz), 6.408 (d, 1H, J=8.4 Hz), 6.35...
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