Muscarinic receptor agonists that are effective in the treatment of pain, alzheimer's disease and schizophrenia
A technology of medicinal salts and enantiomers, which is applied in the field of muscarinic receptor agonists, and can solve the problems that muscarinic agonists and ACHE-Is are not widely used in clinical practice
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Embodiment 1
[0264] Example 1: 4-[(cis (+ / -))-2-oxooctahydro-1H-benzimidazol-1-yl]-1,4'-bipiperidine-1'-ethyl carboxylate
[0265]
[0266] To a solution of racemic (cis)-1-piperidin-4-yloctahydro-2H-benzimidazol-2-one TFA salt (130 mg, 0.40 mmol) in dichloromethane (4 mL) was added Acetic acid (120 μL), followed by ethyl 4-oxopiperidine-1-carboxylate (120 μL) and NaBH(OAc) 3 (250 mg), and the mixture was stirred overnight at 45°C. Then the mixture was washed with saturated NaHCO 3 The solution was quenched, then diluted in dichloromethane. 1N NaOH was added and the aqueous phase was extracted several times with dichloromethane. The combined organic phases were dried and concentrated in vacuo. The compound was purified by high pH preparative LCMS to afford the title compound (25 mg). 1 H NMR (400MHz, chloroform-D): δ ppm 1.09-1.19(m, 1H), 1.23(t, J=7.16Hz, 3H), 1.29-1.46(m, 3H), 1.45-1.91(m, 12H) , 2.13-2.32(m, 2H), 2.33-2.46(m, 1H), 2.62-2.77(m, 2H), 2.88(d, J=12.69Hz, 1H), 2.93(...
Embodiment 8
[0293] Example 8: (trans (+ / -))-1-{1-[1-(cyclopentylcarbonyl)pyrrolidin-3-yl]piperidin-4-yl}octahydro-2H-benzimidazole -2-one
[0294]
[0295] Step 1: Preparation of 3-{4-[(trans(+ / -))-2-oxooctahydro-1H-benzimidazol-1-yl]piperidin-1-yl}pyrrolidine-1-carboxylic acid tert-butyl ester
[0296]
[0297] Following a procedure similar to that described in Example 1, 3-{4-[(trans(+ / -))-2-oxooctahydro-1H-benzimidazol-1-yl]piperidine-1 was prepared -Yl}pyrrolidine-1-carboxylic acid tert-butyl ester (2.40 g), as a mixture of diastereomers.
[0298] Step 2: Preparation of 3-{4-[(trans(+ / -))-2-oxooctahydro-1H-benzimidazol-1-yl]piperidin-1-yl}pyrrolidine
[0299]
[0300] The crude intermediate from step 1 (2.4 g) was dissolved in dichloromethane (10 mL) and TFA (5 mL) was added. The reaction mixture was stirred overnight at room temperature. Removal of solvent and excess TFA gave the title compound as its TFA salt (4.2 g). Conversion of the TFA salt to its free base by MP ...
preparation Embodiment 9-13
[0305]
PUM
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