1257220-43-1|7,7-Dimethyl-5-phenyl-5,7-dihydroindeno[2,1-b]carbazole| Ambeed

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CAS No. :	1257220-43-1
Formula :	C₂₇H₂₁N
M.W :	359.46
SMILES Code :	CC(C1=CC(N(C2=CC=CC=C2)C3=C4C=CC=C3)=C4C=C15)(C)C6=C5C=CC=C6

Yield	Reaction Conditions	Operation in experiment
97%	With tris-(dibenzylideneacetone)dipalladium(0); tri-tert-butyl phosphine; sodium t-butanolate; In toluene; for 12h;Reflux;	100 g (353 mmol) of indenocarbazole, A suspension of 5 mL (529 mmol) of iodobenzene, 16 g (17 mmol) of Pd2(dba)3, 17 mL (35 mmol) of tri-tert-butylphosphine and 102 g (1,059 mmol) of sodium tertiary butoxide was suspended in 1,500 mL of toluene Followed by reflux stirring for 12 hours. The mixture was extracted with dichloromethane and distilled water, and the organic layer was subjected to silica gel filtration. The organic solution was removed and silica gel column was obtained to obtain 124 g (yield: 97%) of 1,1-dimethyl-3-phenyl-1,3-dihydroindeno [2,1- b] carbazole.
88.3%	With 3,5-ditertbutyl salicylic acid; copper; potassium carbonate; sodium hydrogensulfite; at 170℃; for 10h;Inert atmosphere;	The resulting <strong>[1257220-47-5]12,12-dimethyl-10,12-dihydroindeno[2,1-b]carbazole</strong> (7.8 g), iodobenzene (3.7 ml), sodium bisulfite (0.43 g), a copper powder (0.17 g), 3,5-di(tert-butyl)salicylic acid (0.69 g), potassium carbonate (5.71 g), and dodecylbenzene (10 ml) were added to a nitrogen-substituted reaction vessel, heated, and stirred at 170C for 10 hours. The mixture was cooled to 100C, extracted by adding toluene (100 ml), concentrated under reduced pressure, and crystallized using n-hexane (30 ml) to obtain a pale yellow powder of 12,12-dimethyl-10-phenyl-10,12-dihydroindeno[2,1-b]carbazole (8.73 g; yield 88.3%).
88.3%	With 3,5-ditertbutyl salicylic acid; copper; potassium carbonate; sodium hydrogensulfite; at 170℃; for 10h;Inert atmosphere;	The obtained 12,12-dimethyl-10,12-indan[2,1-b]carbazole 7.8g,With 3.7ml of benzene iodide, 0.43g of sodium bisulfite, 0.17g of copper powder,3,5-bis(tert-butyl)salicylic acid 0.69g, potassium carbonate 5.71g,Dodecylbenzene 10ml,Add to the nitrogen-replaced reaction vessel and heat,Stir at 170C for 10 hours. Cool to 100C,After adding 100ml of toluene for extraction, it was concentrated under reduced pressure.Furthermore, 30ml of n-hexane was used for crystallization to obtainThe lightness of 12,12-dimethyl-10-phenyl-10,12-indan[2,1-b]carbazole8.73g yellow powder (yield 88.3%).

Yield	Reaction Conditions	Operation in experiment
91%	With bis(tri-t-butylphosphine)palladium(0); sodium t-butanolate; In 5,5-dimethyl-1,3-cyclohexadiene; for 10.5h;Reflux;	After dissolving 15.0 g (1.0 eq) of formula A1, 9.1 g (1.1 eq) of bromobenzene 2a and 6.6 g (1.3 eq) of NaOt-Bu in 150 ml of xylene,0.81 g (0.03 eq) of bis (tri-tert-butylphosphine) palladium (0) was added and the mixture was refluxed and stirred. After 10.5 hours, lower the temperature to room temperature, filter and wash with water to remove the base. 17.3 g (yield: 91%) of Intermediate A-3 was obtained using chloroform and ethyl acetate.
85.2%	With tris-(dibenzylideneacetone)dipalladium(0); tri-tert-butyl phosphine; sodium t-butanolate; In toluene; at 110 - 120℃;Inert atmosphere;	(3) In a 250mL three-neck flask, under the protection of nitrogen, add 0.02mol intermediate T-2-1, 0.03mol bromobenzene, 0.05mol sodium tert-butoxide, 0.2mmol Pd2(dba)3, 0.2mmol tri-tert-butyl phosphine, stir and mix with 150mL toluene, heat to 110-120 C, reflux for 12-24 hours,The sampling point board shows that there is no intermediate T-2-1 remaining, and the reaction is complete; naturally cool to room temperature, filter,The filtrate was rotary evaporated under reduced pressure to no fraction, and passed through a neutral silica gel column to obtain intermediate T-3-1; HPLC purity 94.8%, yield 85.2%;
77.9%	With tris-(dibenzylideneacetone)dipalladium(0); tri-tert-butyl phosphine; sodium t-butanolate; In toluene; at 110 - 120℃;Inert atmosphere;	(3) In a 250 mL three-neck flask, under the protection of nitrogen, add 0.02mol of intermediate S2-10.03mol raw material E-1,0.05mol sodium tert-butoxide, 0.2mmolPd2 (dba) 3,0.2mmol of tri-tert-butylphosphine was stirred and mixed with 150mL of toluene, heated to 110-120 C, and reacted at reflux for 12-24 hours. The sampling point showed no intermediate S2-1 remaining and the reaction was complete; naturally cooled to room temperature and filtered The filtrate was rotary evaporated under reduced pressure to no fractions and passed through a neutral silica gel column to obtain intermediate S3-1; the purity by HPLC was 98.7% and the yield was 77.9%;

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CAS No.: 1257220-43-1

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CAS No.: 1257220-43-1

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[ 1257220-43-1 ] 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