Home Cart Sign in  
Chemical Structure| 66504-62-9 Chemical Structure| 66504-62-9

Structure of 66504-62-9

Chemical Structure| 66504-62-9

*Storage: {[sel_prStorage]}

*Shipping: {[sel_prShipping]}

,{[proInfo.pro_purity]}

4.5 *For Research Use Only !

{[proInfo.pro_purity]}
Cat. No.: {[proInfo.prAm]} Purity: {[proInfo.pro_purity]}

Change View

Size Price VIP Price

US Stock

Global Stock

In Stock
{[ item.pr_size ]} Inquiry {[ getRatePrice(item.pr_usd,item.pr_rate,item.mem_rate,item.pr_is_large_size_no_price, item.vip_usd) ]}

US Stock: ship in 0-1 business day
Global Stock: ship in 5-7 days

  • {[ item.pr_size ]}

In Stock

- +

Please Login or Create an Account to: See VIP prices and availability

US Stock: ship in 0-1 business day
Global Stock: ship in 2 weeks

  • 1-2 Day Shipping
  • High Quality
  • Technical Support
Product Citations

Alternative Products

Product Details of [ 66504-62-9 ]

CAS No. :66504-62-9
Formula : C10H8ClF3O2
M.W : 252.62
SMILES Code : O=C(OC)CC1=CC=C(Cl)C(C(F)(F)F)=C1
MDL No. :MFCD25965957

Safety of [ 66504-62-9 ]

Application In Synthesis of [ 66504-62-9 ]

* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.

  • Downstream synthetic route of [ 66504-62-9 ]

[ 66504-62-9 ] Synthesis Path-Downstream   1~1

  • 1
  • [ 67-56-1 ]
  • [ 22902-86-9 ]
  • [ 66504-62-9 ]
YieldReaction ConditionsOperation in experiment
With sulfuric acid; at 50℃; for 1h; Carbon tetrabromide (3.48 g, 10.5 mmol) and triphenylphosphine (2.75 g, 10.5 mmol) were added to a solution of [4-chloro-3-(trifluoromethyl)phenyl]methanol (2.00 g, 9.59 mmol) in tetrahydrofuran (12 ml) under ice-cooling, and the mixture was stirred at room temperature for 1 hour. Hexane was added to the reaction mixture, and the insolubles were removed by filtration. The obtained filtrate was poured into water and, after the mixture was extracted with ethyl acetate, the organic layer was successively washed with water and saturated aqueous NaCl solution, and dried over anhydrous sodium sulfate. The residue obtained by evaporating the solvent under reduced pressure was purified by silica gel column chromatography (elution solvent: n-hexane/ethyl acetate=4/1-2/1) to obtain 4-(bromomethyl)-1-chloro-2-(trifluoromethyl)benzene. Potassium cyanide (687 mg, 10.5 mmol) was added to a mixed solution of the obtained 4-(bromomethyl)-1-chloro-2-(trifluoromethyl)benzene in ethanol-water (3:1, 20 ml), and the mixture was stirred at 60C for 2 hours. The reaction mixture was poured into water and, after the mixture was extracted with ethyl acetate, the organic layer was washed with saturated aqueous NaCl solution and dried over anhydrous sodium sulfate. The residue obtained by evaporating the solvent under reduced pressure was subjected to silica gel column chromatography (elution solvent: n-hexane/ethyl acetate=4/1-2/1) to obtain crude [4-chloro-3-(trifluoromethyl)phenyl]acetonitrile. Acetic acid (6 ml) and concentrated hydrochloric acid (6 ml) were added to the obtained crude product, and the mixture was stirred at 100C for 2 hours. After the temperature of the reaction mixture was returned to room temperature, the mixture was poured into water, and the mixture was extracted with ethyl acetate. The organic layer was successively washed with water and saturated aqueous NaCl solution, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure to obtain crude <strong>[22902-86-9][4-chloro-3-(trifluoromethyl)phenyl]acetic acid</strong>. Methanol (12 ml) and concentrated sulfuric acid (1.0 ml) were added to the obtained crude product, and the mixture was stirred at 50C for 1 hour. The temperature of the reaction mixture was returned to room temperature, and the solvent was evaporated under reduced pressure. After ethyl acetate was added thereto, the organic layer was successively washed with water, saturated aqueous sodium hydrogencarbonate solution and saturated aqueous NaCl solution, and dried over anhydrous sodium sulfate. The residue obtained by evaporating the solvent under reduced pressure was purified by silica gel column chromatography (elution solvent: n-hexane/ethyl acetate=10/1) to obtain methyl [4-chloro-3-(trifluoromethyl)phenyl]acetate (1.08 g, two steps total yield: 45%). 1H-NMR (400MHz, CDCl3) : delta 7.58 (1H, d, J = 2.0 Hz), 7.45 (1H, d, J = 8.0 Hz), 7.37 (1H, dd, J = 8.0, 2.0 Hz), 3.70 (3H, s), 3.64 (2H, s).
 

Historical Records