background and overview[1]
2-di-tert-butylphosphine-1-phenylindole can be used as a pharmaceutical synthesis intermediate and an organic intermediate. it is mainly used in laboratory research and development processes and chemical and pharmaceutical synthesis processes. if 2-di-tert-butylphosphine-1-phenylindole is inhaled, move the patient to fresh air; if skin contact occurs, remove contaminated clothing and rinse skin thoroughly with soap and water. if discomfort occurs , seek medical attention; if eye contact occurs, separate eyelids, rinse with running water or saline, and seek medical attention immediately; if ingested, rinse mouth immediately, do not induce vomiting, and seek medical attention immediately.
preparation[1]
2-di-tert-butylphosphine-1-phenylindole is prepared as follows:
a) synthesis of n-phenylindole
place 0.19g (0.1mmol) of cui, 2.34g (20mmol) of 1, 8.82g (42mmol) of k3po4, 0.48ml (4mmol) of 1,2-diaminocyclohexane and 3.16ml (30mmol) 2 was stirred in 20 ml dry dioxane at 110 °c for 24 h. the mixture was then diluted with 50 ml of ethyl acetate. the purple precipitate was filtered through silica gel, resulting in a yellow solution, which was concentrated under vacuum (20 mbar, 50°c). the remaining orange oil was purified by column chromatography (silica gel, hexane/ethyl acetate 98/2). yield: 3.0g (15.5mmol; 75%).
b) synthesis of n-phenyl-2-(di-tert-butylphosphino)indole (2-di-tert-butylphosphine-1-phenylindole)
add 1.6ml (15mmol) of tmeda to 1.93g (10mmol) dissolved in 30ml of hexane. a solution of n-buli (6.25 ml, 10 mmol) (1.6 m in hexane) was added dropwise. after 3 hours of reflux (75°c), the color deepened from yellow to orange. without cooling, a solution of 2.2 ml (10 mmol) chlorodi-tert-butylphosphine in 20 ml hexane was added dropwise. after refluxing for another hour, the color of the mixture became lighter again, and a white solid precipitated. after cooling, 30 ml of water was added to the mixture. the aqueous phase was extracted 3 times, using 20 ml of hexane each time. the combined organic phases were washed with 10 ml of water, dried over na2so4 and concentrated in vacuo (45°c). boil the yellow residue in 30 ml meoh for 30 minutes. after cooling to room temperature, the product obtained was filtered off (660 mg, 17%).
main reference materials
[1] cn200480013398.7 nitrogen-containing monodentate phosphine and its application in catalysis
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