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Chemical Structure| 75462-59-8 Chemical Structure| 75462-59-8

Structure of 75462-59-8

Chemical Structure| 75462-59-8

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Product Details of [ 75462-59-8 ]

CAS No. :75462-59-8
Formula : C9H5ClF6
M.W : 262.58
SMILES Code : FC(C1=CC(C(F)(F)F)=CC(CCl)=C1)(F)F
MDL No. :MFCD00009906
Boiling Point : No data available
InChI Key :OINTXXMBRBLMHH-UHFFFAOYSA-N
Pubchem ID :123576

Safety of [ 75462-59-8 ]

GHS Pictogram:
Signal Word:Danger
Hazard Statements:H314
Precautionary Statements:P280-P305+P351+P338-P310
Class:8
UN#:3261
Packing Group:

Application In Synthesis of [ 75462-59-8 ]

* 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 [ 75462-59-8 ]

[ 75462-59-8 ] Synthesis Path-Downstream   1~3

  • 1
  • ethyl acetate n-hexane [ No CAS ]
  • [ 32707-89-4 ]
  • [ 75462-59-8 ]
YieldReaction ConditionsOperation in experiment
59% With triphenylphosphine; In pentane; 4c) Triphenylphosphine (371 mg, 1.41 mmol) was added to a solution of 3,5-bistrifluoromethylbenzyl alcohol (257 mg, 1.05 mmol) in dry CCl4 (2 ml). The mixture was refluxed for 1 h, then cooled to room temp. Pentane (2 ml) was added, and the mixture stirred for a further 5 min., then filtered. The solid was washed with pentane (2 ml), and the filtrate concentrated in vacuo. The crude product was purified by column chromatography ?SiO2: hexane-ethyl acetate 4:1! to give 3,5-bistrifluoromethylbenzyl chloride (162 mg, 59%); TLC (hexane-ethyl acetate 1:1) rf=0.73.
  • 2
  • [ 32707-89-4 ]
  • [ 75462-59-8 ]
YieldReaction ConditionsOperation in experiment
90% With thionyl chloride;N,N-dimethyl-formamide; at -5 - 20℃; for 7.75h; Preparation of the 3,5-bis(trifluoromethyl*)-benzyl chloride 922.3 g of thionyl chloride (7.752 moles) are placed in a two-litre glass flask provided with mechanical stirring, thermometer, refrigerant, heated metering funnel and brine bath at 07+5C, and 152.0 g of anhydrous DMF are added in portions, under stirring. The solution is cooled at -5/0C by means of a brine bath. 3,5- bis(trifluoromethyl)-benzyl alcohol (1015.0 g, 4.072 moles) are added, keeping the mixture under stirring at a controlled temperature <10C. The metering is completed in approximately 2 hours 45 minutes. The mixture is left under stirring at 200C a further 5 hours to complete the reaction. The GC control at this point indicates a conversion >99.5% and a titer in 3,5-bis(trifluoromethyl)-benzyl chloride equal to 96.6%. The mass is brought to 500C and the two phases are separated: 1352.8 g of yellow organic phase (lower phase) and 424.4 g of thionyl/DMF mixture are obtained. The organic phase is neutralised by two basic aqueous washing operations <n="7"/>(10% solution of NaHCCbeta), in the cooled flask with a water/ice bath and after separation a further washing operation is performed with 10% NaOH at 5O0C (1251.0 g). 1010.7 g of raw product are separated and purified by distillation.Conversion (GC % area): >99.5% Molar yield: 90%GC titer of the 3,5-bis(trifluoromethyl)-benzyl chloride (% area): 99.2% min.
  • 3
  • [ 75462-59-8 ]
  • [ 436-77-1 ]
  • C64H54F18N2O6(2+)*2Cl(1-) [ No CAS ]
YieldReaction ConditionsOperation in experiment
11.05g With diethylamine; In dichloromethane; at 0℃; for 72h; Weigh 6.10g of <strong>[436-77-1]fangchinoline</strong>base dissolved in 100mL of dichloromethane in a 500mL three-necked flask.Add diethylamine10mL, 3,5-bis(trifluoromethyl)benzyl chloride 8.00g, stirred, and incubated at 0 C for 72h, TLC detection of all reactions of <strong>[436-77-1]fangchinoline</strong>,The methylene chloride was distilled off until the liquid volume was reduced to 50 mL, cooled to 5 C for crystallization overnight, filtered, and the product was separated and purified by TLC, and the solid was dried at 60 C for 4 h.That is, 11.05 g of a product in the form of a yellow powder. The desired product has the melting point: 210.4-212.2 C, 13C NMR (CDCl3, 100 MHz) delta 154.00, 151.41, 151.37, 151.21, 149.148.81,148.69,147.32,143.84,140.85,136.19,135.54,135.47,135.41,135.21,135.01,134.84, 132.75, 131.79, 131.54, 131.46, 131.24, 131.02, 130.84, 130.28, 130.12, 129.86,129.43, 128.73, 128.65, 127.42, 127.31, 124.99, 123.57, 123.34, 123.21, 122.87, 122.87,122.65, 122.57, 122.34, 122.26, 121.55, 120.39, 116.38, 113.29, 111.78, 106.24, 72.50,64.03, 61.65, 57.21, 55.84, 45.87, 45.55, 45.48, 44.29, 42.59, 42.37, 42.23, 42.18,38.92, 25.17, 22.35. TOF-HRMS: M/e (1360.0000), molecular formula: C64H54O6N2F18Cl2, that is, compound III20 in Table 2.
 

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