반응 #1256727

ord-7ce447b2f5354f6cadf3fecd2ba93098

반응 방정식

ClB1NB(Cl)NB(Cl)N1
B,B′,B″-trichloroborazine
CCCCCCN
n-hexyl amine
CCN(CC)CC
triethyl amine
CCCCCCNB1NB(NCCCCCC)NB(NCCCCCC)N1
B,B′,B″-tris(hexylamino)borazine
수율 97.3%

반응 조건

온도
60°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONAfter completion of the drop-wise addition
  2. 2
    기타An amine-HCl salt generated was removed by filtration
  3. 3
    기타followed by removal of the solvent and unreacting amine under reduced pressure

실험 절차

B,B′,B″-trichloroborazine (15 g) was dissolved into sufficiently dewatered toluene (100 mL) and a mixture solution of n-hexyl amine (37 g), triethyl amine (25 g) and toluene (100 mL) was dropped over 1 hour at room temperature. After completion of the drop-wise addition, the solution was stirred at 25° C. for 3 hours and further at 60° C. for 3 hours. An amine-HCl salt generated was removed by filtration, followed by removal of the solvent and unreacting amine under reduced pressure to obtain B,B′,B″-tris(hexylamino)borazine as yellow viscous liquid (30 g). Thus obtained compound was further stirred in xylene at 130° C. for 3 hours to proceed polycondensation reaction. After the reaction, the solvent is removed under reduced pressure to obtain a borazine ring-containing compound 2.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07824784B2uspto-grants-2010_11