Methanesulfonic acid, 1,1,1-trifluoro-, calcium salt (2:1) → 2-(9-Benzenesulfonyl-1,3,4,9-tetrahydro-beta-carbolin-2-yl)-1-(1,4-dioxaspiro[4.5]dec-8-yl)ethanol

Calcium trifluoromethanesulfonate (1.22 g, 3.60 mmol) was added to a solution of the product from stage 3 (2.51 g, 8.05 mmol) and 8-oxiranyl-1,4-dioxaspiro[4.5]decane (1.34 g, 7.30 mmol) in anhydrous tetrahydrofuran (50 ml) and the mixture was stirred at room temperature for 48 h. The tetrahydrofuran was removed i. vac. The residue was taken up in methylene chloride (40 ml) and the mixture was washed with 25% potassium carbonate solution (2×25 ml). The organic phase was dried with sodium sulfate and concentrated i. vac. The crude product (4.31 g) was purified by flash chromatography with cyclohexane/ethyl acetate (1:2).

1. customThe tetrahydrofuran was removed i
2. washthe mixture was washed with 25% potassium carbonate solution (2×25 ml)
3. dry with materialThe organic phase was dried with sodium sulfate
4. concentrationconcentrated i
5. customThe crude product (4.31 g) was purified by flash chromatography with cyclohexane/ethyl acetate (1:2)

ORD-Eintrag

ord-ae64a643ae504c869995656fecd3f845

Quelldatensatz

uspto-grants-2012_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08288406B2