Isopropylethanediol → 2-Isopropoxyethyl Methanesulfonate

温度

0 °C

A round bottom flask was charged with 2-isopropoxyethanol (0.5 mL, 4.34 mmol) and dichloromethane (21.68 mL) and was cooled to 0° C. Triethylamine (1.208 mL, 8.67 mmol) was added along with a tip of DMAP. Methanesulfonyl chloride (0.338 mL, 4.34 mmol) was added dropwise. The reaction mixture was slowly warmed to rt over 2 h. The reaction mixture was quenched with saturated aqueous ammonium chloride and transferred to a separatory funnel. The aqueous layer was extracted with dichloromethane (2×). The combined organics were washed with brine, dried over anhydrous sodium sulfate, filtered and concentrated in vacuo. 2-Isopropoxyethyl methanesulfonate (1 g) was isolated as a clear oil and was immediately used in the next reaction.

1. temperatureThe reaction mixture was slowly warmed to rt over 2 h
2. customThe reaction mixture was quenched with saturated aqueous ammonium chloride
3. customtransferred to a separatory funnel
4. extractionThe aqueous layer was extracted with dichloromethane (2×)
5. washThe combined organics were washed with brine
6. dry with materialdried over anhydrous sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated in vacuo

ORDレコード

ord-5dd2a2d8c64b4e20b81cc5e9e4f85b5f

出典データセット

uspto-grants-2012_06

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08202881B2