Dimethyl Sulfate → 1-Iodo-2-[(methylthio)methyl]-benzene

Temperatur

105 °C

To a mixture of 2-(2-iodo-benzyl)-isothiourea (13.53 g, 36.2 mmol) from previous step and a solution of NaOH (22 mL) in water (15 mL) was added dropwise dimethylsulfate (4.1 mL, 43.4 mmol). The reaction mixture was heated to reflux (105° C.) for 2 h, cooled. The resulting oil was then extracted into diethyl oxyde, the organic layer was washed with water, dried over Na2SO4. On concentration the solution generated a yellow oil that was directly used in the next step without any further purification (8.5 g, yield=89%).

1. temperatureThe reaction mixture was heated
2. temperaturecooled
3. extractionThe resulting oil was then extracted into diethyl oxyde
4. washthe organic layer was washed with water
5. dry with materialdried over Na2SO4
6. concentrationOn concentration the solution
7. customwas directly used in the next step without any further purification (8.5 g, yield=89%)

ORD-Eintrag

ord-1e3f097074eb43ca8f36850b5f394187

Quelldatensatz

uspto-grants-2011_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US07981907B2