1350648-40-6|3,5-Difluoro-4-iodopicolinonitrile| Ambeed

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CAS No. :	1350648-40-6
Formula :	C₆HF₂IN₂
M.W :	265.99
SMILES Code :	N#CC1=NC=C(F)C(I)=C1F
MDL No. :	MFCD22627842

GHS Pictogram:
Signal Word:	Warning
Hazard Statements:	H302-H312-H315-H319-H332-H335
Precautionary Statements:	P261-P264-P270-P271-P280-P301+P312-P302+P352-P304+P340-P305+P351+P338-P330-P332+P313-P337+P313-P362-P403+P233-P405-P501

Yield	Reaction Conditions	Operation in experiment
48%		LDA (841.14 mg, 7.85 mmol, 1.10 equiv) was added dropwise into a solution of 3,5- difluoropyridine-2-carbonitrile (1.00 g, 7.14 mmol, 1.00 equiv) in tetrahydrofuran (15 mL). at -78°C under nitrogen. After being stirred for 30 mm at -78°C a solution of ?2 (1.81 g, 7.13 mmol, 1.00 equiv) in tetrahydrofuran (8 mL) was added dropwise. The resulting reaction was stirred at -78°C for 40 minutes, quenched by water, extracted with ethyl acetate, washed with brine, dried over anhydrous sodium sulfate, and concentrated under vacuum. The residue was purified by a silica gel column eluting with ethyl acetate/petroleum ether (1:5) to afford the title compound (920 mg, 48percent) as a yellow solid.
21%		[0116] Preparation 13: 6-fluoro-7-iodo-lH-pyrazolo[4,3-b]pyridine[0117] THF (42 mL) and diisopropylamine (5.6 ml, 39.27mmol) were combined and cooled at 0 °C then n-butyllithium (17.3 ml, 2.5 M in hexane) was added dropwise at 0°C, and stirred for another 30 minutes. The mixture was then cooled in a dry ice/acetone bath to about -78°C and a solution of <strong>[298709-29-2]3,5-difluoropicolinonitrile</strong> (5 g, 35.7 mmol) in THF (25mL) was slowly added. After 30 minutes a solution of I2 (9g, 35.7 mmol) in THF (35mL) was added. The reaction was stirred for another 40 minutes at -78°C in the dry ice/acetone bath, then warmed slightly and quenched with 50 mL sodium thiosulfate solution (10percent aq) followed by dilution with water and EtOAc (300 mL). The organic layer was washed with brine, dried over sodium sulfate, filtered, and concentrated to a residue which was purified by silica column chromatography eluting with petroleum ether-ethyl acetate (5: 1) to give 3, 5-difiuoro-4-iodopicolinonitrile as a solid (2 g, 21 percent yield). 1H NMR (400 MHz, DMSO- d6) delta ppm 8.58 (s, 1 H).

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P378
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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.
Storage
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P401
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P403 + P235	Store in a well-ventilated place. Keep cool.
P410 + P403	Protect from sunlight. Store in a well-ventilated place.
P410 + P412	Protect from sunlight. Do not expose to temperatures exceeding 50 oC/122oF.
P411 + P235	Keep cool.
Disposal
Code	Phrase
P501	Dispose of contents/container to ...
P502	Refer to manufacturer/supplier for information on recovery/recycling

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CAS No.: 1350648-40-6

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CAS No.: 1350648-40-6

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[ 1350648-40-6 ] Synthesis Path-Downstream 1~1

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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