Anesthetic medicine composition and application thereof
A composition and drug technology, applied in the field of biomedicine, can solve problems such as low potency
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Embodiment 1
[0036] Embodiment 1. Preparation of compound 1
[0037] The first step: 2-(2-isopropylphenoxy)tetrahydropyran (3B)
[0038] Add 2-isopropylphenol (3A) (10.00g, 73.40mmol), 3,4-dihydropyran (18.60g, 220.20mmol) and dichloromethane (50mL) into the reaction flask, stir well and add p Pyridine tosylate (1.86g, 7.40mmol), stirred at room temperature for 20 hours, added water (30mL), extracted with dichloromethane (30mL×3), combined organic phases, washed with saturated brine (30mL×3), anhydrous Dry over sodium sulfate, filter, concentrate the filtrate under reduced pressure, and separate and purify the residue by silica gel column chromatography (petroleum ether / ethyl acetate (v / v)=500:1) to obtain 2-(2-isopropyl phenoxy)tetrahydropyran (3B) (13.4 g, yield: 82.71%, HPLC: 99.15%).
[0039] 1HNMR (400MHz, CDCl 3 ): δ7.25-7.20 (m, 1H), δ7.15-7.09 (m, 2H), δ6.97-6.93 (m, 1H), δ5.44-5.42 (m, 1H), δ3.94- 3.88(m,1H), δ3.65-3.62(m,1H), δ3.39-3.22(m,1H), δ1.90-1.86(m,1H), δ1.73-1.67(m,...
Embodiment 2
[0054] Embodiment 2. Preparation of Compound A
[0055] Add 2-(1-cyclopropylvinyl)-6-isopropylphenol (2.0 g, 10 mmol) and dichloromethane (8 mL) to an autoclave (250 mL) at room temperature, add catalyst ((4R, 5R )-(+)-O-[1-benzyl-1-(5-methyl-2-phenyl-4,5-dihydrooxazol-4-yl)-2-phenylethyl]( Dicyclohexylphosphonite) (1,5-COD) iridium (I) tetrakis (3,5-bis (trifluoromethyl) phenyl borate (17mg, 0.01mmol), hydrogen replacement 3 times, under 40atm Reacted for 6 hours, concentrated, and purified the residue by flash column chromatography (petroleum ether / ethyl acetate (v / v)=10:1) to obtain 2-[(1R)-1-cyclopropylethyl ]-6-isopropyl-phenol (compound A) (1.8 g, yield: 90%; chiral HPLC: 91.2%).
[0056] MS m / z (ESI): 203.1 (M-1).
[0057] 1 HNMR (400MHz, CDCl3): δ7.12(dd, 1H), δ7.07(dd, 1H), 6.89(t, 1H), 6.85(s, 1H), 3.20-3.13(m, 1H), 2.53- 2.46(m, 1H), 1.30(d, 6H), 1.27(d, 3H), 1.08-1.03(m, 1H), 0.58-0.56(m, 1H), 0.47-0.46(m, 1H), 0.22- 0.16 (m, 2H).
Embodiment 3
[0058] Embodiment 3, the preparation of compound B
[0059] Add 2-(1-cyclopropylvinyl)-6-isopropylphenol (102 mg, 0.5 mmol) and dichloromethane (2 mL) to a 250 mL autoclave, add catalyst (4S, 5S)-(-)- O-[1-benzyl-1-(5-methyl-2-phenyl-4,5-dihydrooxazol-4-yl)-2-phenylethyl](dicyclohexylphosphonium)(1 , 5-COD) iridium (I) tetrakis (3,5-bis (trifluoromethyl) phenyl) borate (8.5mg, 0.005mmol), hydrogen replacement three times, reaction at 10atm for 2.5h, concentration, flash column Chromatography (petroleum ether / ethyl acetate (v / v)=10:1) afforded 2-[(1S)-1-cyclopropylethyl]-6-isopropyl-phenol (compound B ) (60 mg, yield: 59%; chiral HPLC: 97.3%).
[0060] MS m / z (ESI): 203.1 (M-1).
[0061] 1 HNMR (400MHz, CDCl3): δ7.12(dd, 1H), δ7.07(dd, 1H), 6.89(t, 1H), 6.85(s, 1H), 3.20-3.13(m, 1H), 2.53- 2.46(m, 1H), 1.30(d, 6H), 1.27(d, 3H), 1.08-1.03(m, 1H), 0.58-0.56(m, 1H), 0.47-0.46(m, 1H), 0.22- 0.16 (m, 2H).
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