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
28 suppliers
$226.00/50mL
109-94-4
492 suppliers
$10.00/10g
1026813-15-9
2 suppliers
inquiry
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
28 suppliers
$226.00/50mL
79099-07-3
0 suppliers
$5.00/5g
849106-39-4
1 suppliers
inquiry