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ChemicalBook CAS DataBase List 9,9'-spirobi[fluoren]-2-amine

9,9'-spirobi[fluoren]-2-amine synthesis

10synthesis methods
Ethanamine, N-[(3,5-dichlorophenyl)methylene]-2,2-diethoxy-

1000210-73-0
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Yield: 91%

Reaction Conditions:

with palladium 10% on activated carbon;hydrogen in isopropyl alcohol at 60; under 2280.15 Torr; for 1 h;

Steps:

1.C (C) Synthesis of 2-amino-9,9'-spirobifluorene: (Compound 3)
The obtained compound 2 (40.5 g) is put into a hydrogen reactor, 500 ml of IPA is added, and the mixture is stirred with RPM 450.At 60 ° CAfter confirming that the compound is completely dissolved, 1 g of Pd-C 10% (wet 50%) is added and H2 (g) is maintained at 3 atm for 1 hour. Filter to remove Pd-C. Concentrate the IPA to about 100 ml, cool it to about 5 ° C, and filter. 100 ml of IPE was added and the mixture was refluxed for 1 hour, cooled at room temperature and filtered to obtain 33.8 g (102 mmol) of the title compound (yield: 91%).

References:

FNG RESEARCH CO., LTD.;GOO, YOUNG-SAM;KIM, JEONG-TAE KR2016/102949, 2016, A Location in patent:Paragraph 0074; 0076; 0077; 0084; 0085