928783-84-0|1,3-Dichloro-2-fluoro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzene| Ambeed

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CAS No. :	928783-84-0
Formula :	C₉H₄Cl₂F₄
M.W :	259.03
SMILES Code :	C=C(C1=CC(Cl)=C(F)C(Cl)=C1)C(F)(F)F
MDL No. :	MFCD27933323

GHS Pictogram:
Signal Word:	Warning
Hazard Statements:	H302-H315-H319
Precautionary Statements:	P501-P270-P264-P280-P302+P352-P337+P313-P305+P351+P338-P362+P364-P332+P313-P301+P312+P330

Yield	Reaction Conditions	Operation in experiment
56%	With bis-triphenylphosphine-palladium(II) chloride; caesium carbonate; In tetrahydrofuran; at 70.0℃; for 4.0h;Sealed tube;	Step 2: Preparation of 1,3-dichloro-2-fluoro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzene A mixture of <strong>[1092485-88-5]2-(3,5-dichloro-4-fluorophenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane</strong> (2.56 g, 8.83 mmol), 2-bromo-3,3,3-trifluoroprop-1-ene (1.85 g, 10.6 mmol), Cs2CO3 (11.5 mL, 2M, 17.7 mmol) and Pd(PPh3)2Cl2 (200 mg) in THF (30 mL) was heated at 70 C. in a sealed tube for 4 h. The mixture was cooled to rt and partitioned between ether and H2O. The aqueous layer was extracted with EA and the combined organic layers were dried over Na2SO4. The solvent was removed under reduced pressure and the crude product was purified by column chromatography on silica gel eluted with hexanes to give 1,3-dichloro-2-fluoro-5-(3,3,3-trifluoroprop-1-en-2-yl)benzene (1.3 g; yield 56%) as colorless oil. 1H NMR (500 MHz, CDCl3): δ 7.412 (d, J=6.5 Hz, 2H), 6.057 (s, 1H), 5.806 (s, 1H) ppm.
47%	With sodium carbonate;bis-triphenylphosphine-palladium(II) chloride; In 1,4-dioxane; water; at 80.0℃; for 18.0h;Reflux;	Preparation 2. 1,3-dichloro-2-fluoro-5-(1,1,1-trifluoroprop-2-en-2-yl)benzeneTo a stirred solution of 2-bromo-3,3,3-trifluoropropene (2.65 g, 15.1 mmol) and <strong>[1092485-88-5]2-(3,5-dichloro-4-fluorophenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane</strong> (2A.1) (4.4 g, 15.1 mmol) in 1,4-dioxane (60 mL) was added Na2CO3 (4.02 g, 38 mmol) and water (20 mL). Next, bis(triphenylphosphine) palladium II chloride (220 mg, 0.3 mmol) was added and the reaction mixture was heated to 80 C. for 18 hours. The reaction mixture was cooled, filtered, and concentrated under reduced pressure to remove dioxane. The residue was diluted with water (100 mL) and extracted with EtOAc (2×125 mL), dried (Na2SO4), and concentrated under vacuum. Crude material was purified on silica gel with 100% heptane to afford the intermediate as a clear oil (1.8 g, 47%). 1H NMR (CDCl3): δ 7.43 (2H), 6.07 (1H), 5.82 (1H).
	With potassium hydroxide;tetrakis(triphenylphosphine) palladium(0); In tetrahydrofuran; 1,2-dimethoxyethane; water; at 75.0℃; for 6.0h;	2-(3,5-Dichloro-4-fiuorophenyl)-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (11.0 g, 37.8 mmol) and 2-bromo-3,3,3-trifluoropropene (8.0 g, 46 mmol) were added to a mixture of tetrahydrofuran (30 niL), ethylene glycol dimethyl ether (30 mL), and 4 M potassium hydroxide aqueous solution (30 mL) in a 200 mL Fisher-Porter sealed tube, followed by the addition of tetrakis(triphenylphosphine)palladium(0) (264 mg, 0.229 mmol). The reaction mixture was heated at 75 C for 6 h. The reaction mixture was then partitioned between ether and water, and the aqueous layer was separated and washed twice with diethyl ether. The combined organic extracts were dried over MgSθ4 and concentrated under reduced pressure. The residual oily solid was purified by chromatography on silica gel by elution with ethyl acetate/hexane to afford the title compound as an oil (8.33 g). 1H NMR (CDCI3) δ 7.40 (d, 2H), 6.04 (s, 1H), 5.79 (s, 1H).

Precautionary Statements-General
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P101	If medical advice is needed,have product container or label at hand.
P102	Keep out of reach of children.
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Prevention
Code	Phrase
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P220	Keep/Store away from clothing/combustible materials.
P221	Take any precaution to avoid mixing with combustibles
P222	Do not allow contact with air.
P223	Keep away from any possible contact with water, because of violent reaction and possible flash fire.
P230	Keep wetted
P231	Handle under inert gas.
P232	Protect from moisture.
P233	Keep container tightly closed.
P234	Keep only in original container.
P235	Keep cool
P240	Ground/bond container and receiving equipment.
P241	Use explosion-proof electrical/ventilating/lighting/equipment.
P242	Use only non-sparking tools.
P243	Take precautionary measures against static discharge.
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P263	Avoid contact during pregnancy/while nursing.
P264	Wash hands thoroughly after handling.
P265	Wash skin thouroughly after handling.
P270	Do not eat, drink or smoke when using this product.
P271	Use only outdoors or in a well-ventilated area.
P272	Contaminated work clothing should not be allowed out of the workplace.
P273	Avoid release to the environment.
P280	Wear protective gloves/protective clothing/eye protection/face protection.
P281	Use personal protective equipment as required.
P282	Wear cold insulating gloves/face shield/eye protection.
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P284	Wear respiratory protection.
P285	In case of inadequate ventilation wear respiratory protection.
P231 + P232	Handle under inert gas. Protect from moisture.
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Response
Code	Phrase
P301	IF SWALLOWED:
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P321
P322
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P342	If experiencing respiratory symptoms:
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P378
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P390	Absorb spillage to prevent material damage.
P391	Collect spillage. Hazardous to the aquatic environment
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P301 + P312	IF SWALLOWED: call a POISON CENTER or doctor/physician IF you feel unwell.
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P302 + P334	IF ON SKIN: Immerse in cool water/wrap in wet bandages.
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P304 + P340	IF INHALED: Remove victim to fresh air and Keep at rest in a position comfortable for breathing.
P304 + P341	IF INHALED: If breathing is difficult, remove victim to fresh air and keep at rest in a position comfortable for breathing.
P305 + P351 + P338	IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do. Continue rinsing.
P306 + P360	IF ON CLOTHING: Rinse Immediately contaminated CLOTHING and SKIN with plenty of water before removing clothes.
P307 + P311	IF exposed: call a POISON CENTER or doctor/physician.
P308 + P313	IF exposed or concerned: Get medical advice/attention.
P309 + P311	IF exposed or if you feel unwell: call a POISON CENTER or doctor/physician.
P332 + P313	IF SKIN irritation occurs: Get medical advice/attention.
P333 + P313	IF SKIN irritation or rash occurs: Get medical advice/attention.
P335 + P334	Brush off loose particles from skin. Immerse in cool water/wrap in wet bandages.
P337 + P313	IF eye irritation persists: Get medical advice/attention.
P342 + P311	IF experiencing respiratory symptoms: call a POISON CENTER or doctor/physician.
P370 + P376	In case of fire: Stop leak if safe to Do so.
P370 + P378	In case of fire:
P370 + P380	In case of fire: Evacuate area.
P370 + P380 + P375	In case of fire: Evacuate area. Fight fire remotely due to the risk of explosion.
P371 + P380 + P375	In case of major fire and large quantities: Evacuate area. Fight fire remotely due to the risk of explosion.
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P401
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Disposal
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P501	Dispose of contents/container to ...
P502	Refer to manufacturer/supplier for information on recovery/recycling

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CAS No.: 928783-84-0

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CAS No.: 928783-84-0

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[ 928783-84-0 ] Synthesis Path-Downstream 1~2

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Physical hazards
Code	Phrase
H200	Unstable explosive
H201	Explosive; mass explosion hazard
H202	Explosive; severe projection hazard
H203	Explosive; fire, blast or projection hazard
H204	Fire or projection hazard
H205	May mass explode in fire
H220	Extremely flammable gas
H221	Flammable gas
H222	Extremely flammable aerosol
H223	Flammable aerosol
H224	Extremely flammable liquid and vapour
H225	Highly flammable liquid and vapour
H226	Flammable liquid and vapour
H227	Combustible liquid
H228	Flammable solid
H229	Pressurized container: may burst if heated
H230	May react explosively even in the absence of air
H231	May react explosively even in the absence of air at elevated pressure and/or temperature
H240	Heating may cause an explosion
H241	Heating may cause a fire or explosion
H242	Heating may cause a fire
H250	Catches fire spontaneously if exposed to air
H251	Self-heating; may catch fire
H252	Self-heating in large quantities; may catch fire
H260	In contact with water releases flammable gases which may ignite spontaneously
H261	In contact with water releases flammable gas
H270	May cause or intensify fire; oxidizer
H271	May cause fire or explosion; strong oxidizer
H272	May intensify fire; oxidizer
H280	Contains gas under pressure; may explode if heated
H281	Contains refrigerated gas; may cause cryogenic burns or injury
H290	May be corrosive to metals
Health hazards
Code	Phrase
H300	Fatal if swallowed
H301	Toxic if swallowed
H302	Harmful if swallowed
H303	May be harmful if swallowed