4-(2-chloroethyl)-1,2-dimethoxybenzene synthesis
- Product Name:4-(2-chloroethyl)-1,2-dimethoxybenzene
- CAS Number:27160-08-3
- Molecular formula:C10H13ClO2
- Molecular Weight:200.66
7417-21-2
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Yield:27160-08-3 100%
Reaction Conditions:
with dichloro sulfoxide in chloroform; for 4 h;Heating / reflux;
Steps:
28.2
The reaction mixture of 2-(3,4-dimethoxyphenyl)ethanoI (6.0 g, 32.8 mmol) and thionyl chloride (19 g, 164 mmol) in chloroform (20 mL) was stirred at reflux for 4 h, concentrated, and partitioned between water and ethyl acetate. The organic layer was washed with NaHCCb and brine, dried over anhydrous sodium sulfate, and concentrated to afford 4-(2-chloroethyl)- 1,2-flim.ethoxybenzene (K) quantitatively (6.6 g).A reaction mixture of 4-(2-chloroethyl)-l,2-dimethoxybenzene (3.6 g, 17.9 mmol), piρerazine-1-carboxylic acid f-butyl ester (4.0 g, 21.5 mmol), K2CO3 (4.97 g, 36 mmol), and NaI (2.7 g, 18 mmol) in DMF (20 mL) was stirred at 800C for 3 h, cooled to room temperature, and partitioned between water and ethyl acetate. The organic layer was washed with water and brine, dried over anhydrous sodium sulfate, and concentrated. The residue was purified by column chromatography to afford 4-[2-(3,4-dimethoxy-phenyl)-ethyl]- piperazine-1-carboxylic acid *-butyl ester (4.8 g, 76%) which was dissolved in 4 N HCl in dioxane. This solution was stirred at room temperature for 4 h, concentrated, and dried in a high vacuum oven to give the title compound quantitatively.
References:
WO2007/89462,2007,A2 Location in patent:Page/Page column 32
15964-79-1
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