130596-60-0|1-Benzyl-4,4-dimethyl-1,4-azasilinane| Ambeed

Yield	Reaction Conditions	Operation in experiment
70%		To a solution of 3 (2.3 g, 10.5 mmol) in ethanol (EtOH), 6 N HC1 (10.5 mmol) is added and the solvent is removed under reduced pressure. The reaction mixture is co-evaporated with EtOH ( 2 X 10 mL ) and recrystallized from EtOH-diethyl ether. To a slurry of Pd/C in EtOH, an ethanolic solution of the HC1 salt is added dropwise and stirred at 25 C under hydrogen atmosphere for 20 h. The reaction mixture is filtered through celite, washed with 2 X 20 mL of Methanol. The filtrate is concentrated under reduced pressure to give a viscous oil which is titrated with diethyl ether to obtain the product 4 as a white solid (950 mg) in 70% yield. This compound was previously documented in WO 2006/ 066872.
70%		To a solution of 3 (2.3 g, 10.5 mmol) in ethanol (EtOH), 6 N HCl (10.5 mmol) is added and the solvent is removed under reduced pressure. The reaction mixture is co-evaporated with EtOH (210 mL) and recrystallized from EtOH-diethyl ether. To a slurry of Pd/C in EtOH, an ethanolic solution of the HCl salt is added dropwise and stirred at 25 C. under hydrogen atmosphere for 20 h. The reaction mixture is filtered through celite, washed with 220 mL of Methanol. The filtrate is concentrated under reduced pressure to give a viscous oil which is titrated with diethyl ether to obtain the product 4 as a white solid (950 mg) in 70% yield. This compound was previously documented in WO 2006/066872.
49.5%	With palladium on activated charcoal; hydrogen; In methanol; at 50℃;	The compound 1-benzyl-4,4-dimethyl-1,4-sipadipine (15.0 g, 68.36 mmol) was dissolved in dry methanol and palladium on charcoal (1.5 g) was added; To 50 C.TLC monitoring reaction is completed.Cooled to room temperature, suction filtered, the filtrate was added dropwise an ice-salt solution of isopropyl alcohol, pH was adjusted to about 1, no solid precipitation.Rotate the solvent to give orange salt.35mL ether beating, suction filtration, 5.6g pink powder.Yield 49.5%

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H200	Unstable explosive
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H204	Fire or projection hazard
H205	May mass explode in fire
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H221	Flammable gas
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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
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Health hazards
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H301	Toxic if swallowed
H302	Harmful if swallowed
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H310	Fatal in contact with skin
H311	Toxic in contact with skin
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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

1-Benzyl-4,4-dimethyl-1,4-azasilinane

CAS No.: 130596-60-0

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[ 130596-60-0 ] Synthesis Path-Downstream 1~1

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