Methyl iodide → 3-Methylcaprolactam

To a solution of azepan-2-one (0.5 g, 4.42 mmol, 1 equiv) in anhydrous THF (20 mL) under nitrogen, was added n-BuLi (4.4 mL, 2.5 M in n-hexane, 11.06 mmol) dropwise at 0° C. The reaction mixture was kept at 0° C. for 2 h, then MeI (0.3 mL, 4.86 mmol) was added. After stirring for 1 h, the mixture was quenched with water and extracted with DCM (2×50 mL). The combined organic layers were dried over anhydrous Na2SO4. After filtration and concentration, the crude product was directly used for the next step without further purification. MS (ESI): 128 (MH+).

1. customthe mixture was quenched with water
2. extractionextracted with DCM (2×50 mL)
3. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
4. filtrationAfter filtration and concentration
5. customthe crude product was directly used for the next step without further purification

ORD-Eintrag

ord-44149ac55fb24e058dd4632cdc8e51fd

Quelldatensatz

uspto-grants-2014_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08772301B2