Acetate → Isoamyl Acetate

1-Butanol, 3 methyl, acetate. Under an atmosphere of argon, acetyl chloride (6.5 ml, 91.8 mmol) was added dropwise to a 0° C. solution of isoamyl alcohol (5 ml, 45.9 mmol), N, N-dimethylpyridine (2.8 g, 23 mmol), and anhydrous pyridine (4.1 ml, 50.5 mol) in dichloromethane (92 ml). The reaction mixture was poured into 100 ml of 0.1 N HCl, and the resulting layers were separated. The organic layer was washed with 50 ml of saturated aqueous ammonium chloride then dried over magnesium sulfate. The organic layer was filtered and concentrated in vacuo to a clear oil. The resulting oil was purified by distillation (bp 134-136° C.) to give isoamyl acetate. 1H NMR (300 MHz, CDCl3) 4.08 (t, 2H, J 6.9), 2.03 (s, 3H), 1.68 (m, 1H), 1.51 (q, 2H, J 6.9), 0.92 (d, 6H, J 6.6).

1. customthe resulting layers were separated
2. washThe organic layer was washed with 50 ml of saturated aqueous ammonium chloride
3. dry with materialthen dried over magnesium sulfate
4. filtrationThe organic layer was filtered
5. concentrationconcentrated in vacuo to a clear oil
6. distillationThe resulting oil was purified by distillation (bp 134-136° C.)

ORDレコード

ord-2213bafc23154883acb230183da6cb34

出典データセット

uspto-grants-2005_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US06911338B2