反应详情

温度

0 °C

To a 0° C. solution of N-methylhydroxylamine hydrochloride (793 mg, 2 eq.) in 20 ml of THF:H2O (1:1) with triethylamine (198 ml, 3.0 eq.) was added 4-(n-pentyl) benzoic acid chloride (1.0 ml, 4.75 mmol). The solution was stirred for 0.5 hour at 0° C. then allowed to warm to room temperature and stir overnight. The reaction mixture was diluted with EtOAc and the organic layer was washed with H2O, 1N HCl (2×), and brine, then dried over anhydrous MgSO4. Concentration in vacuo gave a yellow oil which was flash chromatographed in LPS-1 silica gel eluting with (1:1) hexane/EtOAc. Product containing fractions were concentrated in vacuo to yield title product, 380 mg (37%) as a light yellow oil.

1. temperatureto warm to room temperature
2. stirringstir overnight
3. washthe organic layer was washed with H2O, 1N HCl (2×), and brine
4. dry with materialdried over anhydrous MgSO4
5. concentrationConcentration in vacuo
6. customgave a yellow oil which
7. customchromatographed in LPS-1 silica gel eluting with (1:1) hexane/EtOAc
8. additionProduct containing fractions
9. concentrationwere concentrated in vacuo