Ethyl 2-chloropropionate → Ethyl 2-(methylsulfonyl)propanoate

温度

77 °C

Sodium methyl sulfinate (103 g, 937 mmol) was combined with the ethyl 2-chloropropionate (109 g, 892 mmol) in ethanol (350 mL) in a 500 mL one neck round bottom flask. The reaction was heated to 77° C. for 20 h, and then allowed to cool to room temperature. Solids were removed by filtration through celite, and the filter pad was washed with ethanol. The combined filtrates were concentrated under reduced pressure. The crude product was suspended in diethyl ether (250 mL), and solids were removed by filtration. The filtrate was concentrated under reduced pressure to afford the title compound as a pale yellow oil (51 g, 73%). 1H NMR (400 MHz, CHLOROFORM-d) δ1.32 (t, J=7.05 Hz, 3H) 1.67 (d, J=7.47 Hz, 3H) 3.05 (s, 3H) 3.83-3.92 (m, 1H) 4.18-4.37 (m, 2H).

1. temperatureto cool to room temperature
2. customSolids were removed by filtration through celite
3. washthe filter pad was washed with ethanol
4. concentrationThe combined filtrates were concentrated under reduced pressure
5. customsolids were removed by filtration
6. concentrationThe filtrate was concentrated under reduced pressure

ORDレコード

ord-5d79a1cecebb4c3a8ba91f76b9533d09

出典データセット

uspto-grants-2014_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08748466B2