Piperidine → Piperidine, 1-(isocyanoacetyl)-

To stirred and cooled (0° C.) methyl 2-isocyanoacetate (96% technical grade, 2.46 g, 24.63 mmol) was slowly added piperidine (3.22 mL, 37.85 mmol). The mixture was stirred for 1 h with continuous stirring at room temperature and then concentrated. The residue was dissolved in dichloromethane (50 mL) and the organic layer was washed with 10% aqueous citric acid (2×25 mL), dried over MgSO4, filtered and evaporated. 2-Isocyano-1-(piperidin-1-yl)ethanone, SLA 07116B, was obtained as an orange solid (3.13 g, 83% yield) that was used in the next step without further purification.

1. stirringThe mixture was stirred for 1 h
2. stirringwith continuous stirring at room temperature
3. concentrationconcentrated
4. dissolutionThe residue was dissolved in dichloromethane (50 mL)
5. washthe organic layer was washed with 10% aqueous citric acid (2×25 mL)
6. dry with materialdried over MgSO4
7. filtrationfiltered
8. customevaporated

ORDレコード

ord-6f75bf929c60479f8b640f1ed717ad4e

出典データセット

uspto-grants-2012_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08168631B2