2,4-Dichlorophenol → 2,4-Dichloro-1-methylsulfanylmethoxy-benzene

To a solution of 2,4-dichloro-phenol (10 g, 61.35 mmol) in dry DMF (100 mL) was added NaH (2.06 g, 85.89 mmol, 60% in mineral oil). The mixture was stirred for 30 min. at room temperature followed by dropwise addition of chloro-methylsulfanyl-methane (5.65 mL, 67.48 mmol) and stirring was continued for 16 hrs at ambient temperature. The reaction was quenched by addition of water (150 mL) and extracted with diethyl ether (2×100 mL). The combined organic phases were washed with saturated aq. ammonium chloride (2×100 mL), dried (Na2SO4), filtered and evaporated in vacuo afforded 17 g crude 2,4-dichloro-1-methylsulfanylmethoxy-benzene which was used without further purification in the next step.

1. stirringstirring
2. waitwas continued for 16 hrs at ambient temperature
3. customThe reaction was quenched by addition of water (150 mL)
4. extractionextracted with diethyl ether (2×100 mL)
5. washThe combined organic phases were washed with saturated aq. ammonium chloride (2×100 mL)
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. customevaporated in vacuo

ORDレコード

ord-68fb43f11c394765b18bc480b9bf90e0

出典データセット

uspto-grants-2013_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08383683B2