22246-84-0|8-Hydroxy-1,3,4,5-tetrahydro-2H-benzo[b]azepin-2-one| Ambeed

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CAS No. :	22246-84-0
Formula :	C₁₀H₁₁NO₂
M.W :	177.20
SMILES Code :	O=C1NC2=CC(O)=CC=C2CCC1
MDL No. :	MFCD22571424

Yield	Reaction Conditions	Operation in experiment
76%	With boron tribromide; In 4-(dicyanomethylene)-2-methyl-6-(p-dimethylaminostyryl)-4H-pyran;	Example 33 8-Hydroxy-2,3,4,5-tetrahydro-1H-1-benzazepine-2-one To a solution of <strong>[22246-83-9]8-methoxy-2,3,4,5-tetrahydro-1H-1-benzazepine-2-one</strong> (1.00 g, 5.23 mmol) in DCM (5 mL) was added dropwise 1M solution of BBr3 in DCM (5.23 mL). After stirring at room temperature for 30 min, the reaction mixture was heated at reflux for 5 hrs, allowed to cool to ambient temperature and poured into ice-water. The aqueous layer was extracted with DCM (5*10 mL), dried over Na2SO4, filtered and evaporated. The solid residue was washed with n-hexane and dried in high vacuum. The title compound was obtained as a white powder (705 mg, 76%). M.P.: 226-227 C.; MS (FAB): calcd for C10H11NO2 177.2; found m/e 178 (M+1)+. This product was also analyzed by 1H and 13C NMR. The corresponding NMR spectra were consistent with the structure of the anticipated product.
	With boron tribromide; In dichloromethane; at -78 - 20℃; for 16h;	A solution of 8-Methoxy-l,3,4,5-tetrahydro-benzo[b]azepin-2-one (56) (1.1 g, 5.8 mmol) in dichloromethane (60 mL) was cooled to -78 C, and a 1.0 M solution of boron tribromide (12.6 mL, 12.6 mmol) in dichloromethane was added dropwise. The reaction mixture was allowed to warm to room temperature and stir overnight. After 16 h, the reaction mixture was poured into ice/water (30 mL) mixture and stirred vigorously to evaporate the dichloromethane. The solids obtained were filtered, washed with water, and dried to afford the title compound (57) as a tan solid: 1H NMR (CD3OD) δ 7.03 (d, J = 8.2 Hz, IH), 6.57 (dd, J = 8.2, 2.5 Hz, IH), 6.47 (d, J = 2.4 Hz, IH), 2.66 (t, J = 7.0 Hz, 2H), 2.26 (t, J = 6.9 Hz, 2H), 2.16 (t, J= 7.0 Hz, 2H); MS (ESI) m/z 178 [C10Hi1NO2 + H]+.

Precautionary Statements-General
Code	Phrase
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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.
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P265	Wash skin thouroughly after handling.
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P284	Wear respiratory protection.
P285	In case of inadequate ventilation wear respiratory protection.
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Response
Code	Phrase
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P320
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P321
P322
P330	Rinse mouth.
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P378
P380	Evacuate area.
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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 + P350	IF ON SKIN: Gently wash with plenty of soap and water.
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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:
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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
P402	Store in a dry place.
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P422
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Disposal
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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
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H225	Highly flammable liquid and vapour
H226	Flammable liquid and vapour
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H228	Flammable solid
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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
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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
H304	May be fatal if swallowed and enters airways
H305	May be harmful if swallowed and enters airways
H310	Fatal in contact with skin
H311	Toxic in contact with skin
H312	Harmful in contact with skin
H313	May be harmful in contact with skin
H314	Causes severe skin burns and eye damage
H315	Causes skin irritation
H316	Causes mild skin irritation
H317	May cause an allergic skin reaction
H318	Causes serious eye damage
H319	Causes serious eye irritation
H320	Causes eye irritation
H330	Fatal if inhaled
H331	Toxic if inhaled
H332	Harmful if inhaled
H333	May be harmful if inhaled
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H336	May cause drowsiness or dizziness
H340	May cause genetic defects
H341	Suspected of causing genetic defects
H350	May cause cancer
H351	Suspected of causing cancer
H360	May damage fertility or the unborn child
H361	Suspected of damaging fertility or the unborn child
H361d	Suspected of damaging the unborn child
H362	May cause harm to breast-fed children
H370	Causes damage to organs
H371	May cause damage to organs
H372	Causes damage to organs through prolonged or repeated exposure
H373	May cause damage to organs through prolonged or repeated exposure
Environmental hazards
Code	Phrase
H400	Very toxic to aquatic life
H401	Toxic to aquatic life
H402	Harmful to aquatic life
H410	Very toxic to aquatic life with long-lasting effects
H411	Toxic to aquatic life with long-lasting effects
H412	Harmful to aquatic life with long-lasting effects
H413	May cause long-lasting harmful effects to aquatic life
H420	Harms public health and the environment by destroying ozone in the upper atmosphere

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CAS No.: 22246-84-0

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CAS No.: 22246-84-0

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