Methyl 2,4-dichlorophenylacetate synthesis
- Product Name:Methyl 2,4-dichlorophenylacetate
- CAS Number:55954-23-9
- Molecular formula:C9H8Cl2O2
- Molecular Weight:219.06
19719-28-9
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74-88-4
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55954-23-9
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Yield: 100%
Reaction Conditions:
with potassium carbonate in N,N-dimethyl-formamide at 20; for 21 h;
Steps:
5
Reference Example-5
After 2-(2,4-Dichlorophenyl) acetic acid (9.86 g, 48.1 mmol) was dissolved in DMF (50 mL), potassium carbonate (6.65 g, 48.1 mmol) was added thereto, and methyl iodide (21.6 g, 144 mmol) was added thereto, followed by stirring at room temperature for 21 hours.
After the reaction was completed, 2N hydrochloric acid (100 mL) was added to the reaction solution, and the resultant product was extracted with ethyl acetate (50 mL*1, 30 mL*2).
The organic layer was washed with a saturated saline solution (10 mL), dried over anhydrous magnesium sulfate, and concentrated under reduced pressure, whereby a brown oily crude product (15.1 g) was obtained.
This was purified by silica gel column chromatography (hexane:ethyl acetate=5:1), whereby methyl 2-(2,4-dichlorophenyl) acetate (10.7 g, yield: quantitative) was obtained as a colorless oily material. 1H-NMR (400 MHz, CDCl3): δ3.72 (s, 3H), 3.75 (s, 2H), 7.22 (d, J=1.2 Hz, 2H), 7.41 (t, J=1.2 Hz, 1H).
References:
KAKEN PHARMACEUTICAL CO., LTD.;SAGAMI CHEMICAL RESEARCH INSTITUTE;KOBAYASHI, Osamu;NIIKURA, Naoko;INOUE, Tomoko;MIZUTA, Satoshi;TAKATSUNA, Reiko;HIRAI, Kenji;SHIROUZU, Kentaro;OBATA, Miyoo US2016/24110, 2016, A1 Location in patent:Paragraph 0430; 0431
67-56-1
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19719-28-9
373 suppliers
$7.00/10g
55954-23-9
119 suppliers
$9.00/5g