Triethylamine → 6-Methoxy-1-[1-(1-methyl-1H-imidazole-4-sulfonyl)-piperidin-4-yl]-3,4-dihydro-isoquinoline

To a stirred solution of 6-methoxy-1-piperidin-4-yl-3,4-dihydro-isoquinoline (0.094 g, 0.385 mmol) and triethylamine (0.078 g, 0.77 mmol) in CH2Cl2 (3 ml) was added 1-methyl-1H-imidazole-4-sulfonyl chloride (0.070 g, 0.385 mmol). The reaction mixture was stirred at RT under an atmosphere of N2 overnight. The reaction mixture was diluted with CH2Cl2 (10 ml) and washed with water (2×5 ml). The organic layer was dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified via radial chromatography (SiO2, 1 mm, CH2Cl2 to 5% MeOH/CH2Cl2) to give the product as an oil (0.084 g, 0.216 mmol, 56% yield).

1. washwashed with water (2×5 ml)
2. dry with materialThe organic layer was dried over MgSO4
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. customThe residue was purified via radial chromatography (SiO2, 1 mm, CH2Cl2 to 5% MeOH/CH2Cl2)

ORD-Eintrag

ord-88f163b020a4417a8afec3291f8f5e4c

Quelldatensatz

uspto-grants-2003_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06608203B2