4-CHLORO-2-METHYLPHENYLMAGNESIUM BROMID& synthesis
- Product Name:4-CHLORO-2-METHYLPHENYLMAGNESIUM BROMID&
- CAS Number:480438-47-9
- Molecular formula:C7H6BrClMg
- Molecular Weight:229.7845
480438-47-9
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Yield:1026813-15-9 46%
Reaction Conditions:
in tetrahydrofuran at -78 - 20; for 18 h;
Steps:
33.1 Step 1 : Preparation of bis(4-chloro-2-meth l hen l)methanol
A round bottom flask was charged with a 4-chloro-2-methylphenyl magnesium bromide solution (10 mL of a 0.5 M THF solution, 5 mmol, ) and THF (50 mL). The solution was cooled to -78 °C and an ethyl formate solution (200 μ, 2.50 mmol, in 10 mL THF) was added drop wise. The reaction was allowed to stir at -78 °C for 15 min and allowed to warm to room temperature slowly and stirred for 18 hrs. The reaction was diluted in EtOAc and washed with brine (3X). The organics were dried ( a2S04), filtered, and concentrated under reduced pressure. The residue was chromatographed on a silica gel column (hexanes to 15% EtOAc in hexanes) and yielded bis(4-chloro-2-methylphenyl)methanol (643 mg, 46%) as a clear cyrstaline solid. XH NMR 400 MHz (CDC13) δ 7.25 - 7.14 (m, 6H), 6.07 (s, 1H), 2.26 (s, 6H), 1.57 (s, 2H). LCMS (ESI, m/z): 263 [M+H]+.
References:
WO2013/103973,2013,A1 Location in patent:Paragraph 00163
480438-47-9
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