(3S)-N-(L-aminoacyl)-1,2,3,4-tetrahydroisoquinoline-3-carboxylic acid, preparation method and uses thereof
A technology of tetrahydroisoquinoline and glycyl, which is applied in the field of biomedicine, can solve the problems of low solubility, low bioavailability, complicated preparation process, poor solubility, etc., and achieves good thrombolytic activity, high bioavailability, good solubility and the like. The effect of antithrombotic activity
- Summary
- Abstract
- Description
- Claims
- Application Information
AI Technical Summary
Problems solved by technology
Method used
Image
Examples
Embodiment 1
[0041] To 5.0g (0.03mmol) L-phenylalanine, first add 27ml formaldehyde dropwise, and then add 45ml concentrated hydrochloric acid dropwise. The resulting suspension was heated in an oil bath to 80-90°C and stirred for 10 h, TLC (CCl 3 :CH 3OH=10:1) shows the disappearance of phenylalanine. The reaction mixture was cooled to room temperature and filtered. The filter cake was washed with water (30ml×3) and then with acetone (30ml×3) to obtain 4.5g (83.9%) of the title compound as a colorless solid. Mp.302-303; ESI-MS (m / e) 178 [M+H] + ; 1 HNMR (CDCl 3 -d) δ / ppm=11.0(s, 1H), 7.0(m, 4H), 3.80(m, 3H), 3.03(d.1H), 2.78(d, 1H), 2.0(s, 1H); 13 C-NMR (CDCl 3 -d) δ / ppm=174.9, 136.2, 134.2, 127.2, 126.0, 57.6, 47.4, 29.4.
[0042] Example 2 Preparation of (3S)-1,2,3,4-tetrahydroisoquinoline-3-carboxylic acid methyl ester
Embodiment 2
[0043] Add 5.2ml of thionyl chloride dropwise to 20ml of methanol in an ice-salt bath, and stir for 10min after the dropping. Afterwards, 4.27 g (20 mmol) of (3S)-1,2,3,4-tetrahydroisoquinoline-3-carboxylic acid were added. The reaction mixture was stirred at room temperature for 100 h, TLC (CCl 3 :CH 3 OH=5:1) shows the disappearance of (3S)-1,2,3,4-tetrahydroisoquinoline-3-carboxylic acid. The reaction mixture was concentrated under reduced pressure. The residue was dissolved in 20 ml of methanol and concentrated under reduced pressure. This operation was repeated 3 times. The residue was dissolved in 20 ml of ether and concentrated under reduced pressure. This operation was repeated 3 times. The residue was crystallized from methanol / ether to afford 4.2 g (92%) of the title compound as a colorless solid. ESI-MS(m / e)192[M+H] + ; 1 HNMR (CDCl 3 -d) δ / ppm=7.0(m, 4H), 3.80(m, 3H), 3.67(s, 3H), 3.13(d.1H), 2.78(d, 1H), 2.0(s, 1H); 13 C-NMR (CDCl 3 -d) δ / ppm = 174.9, ...
Embodiment 3
[0045] Example 4 Preparation of (3S)-N-(Boc-glycyl)-1,2,3,4-tetrahydroisoquinoline-3-carboxylic acid methyl ester (1b)
PUM
Login to View More Abstract
Description
Claims
Application Information
Login to View More 