تفاعل #2028937

ord-02c8b15a9dad4a318dd81a2cb77af2ea

معادلة التفاعل

CC1(C)c2cccc(P(c3ccccc3)c3ccccc3)c2Oc2c(P(c3ccccc3)c3ccccc3)cccc21
Xantphos
Clc1cc(-c2ccnc(Cl)c2)ccn1
2,2′-dichloro-[4,4′]-bipyridinyl
COCC(C)N
2-amino-1-methoxypropane
CC(C)(C)[O-].[Na+]
sodium tert-butoxide
COCC(C)Nc1cc(-c2ccnc(Cl)c2)ccn1
(2′-Chloro-[4,4′]bipyridinyl-2-yl)-(2-methoxy-1-methyl-ethyl)-amine

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGThe mixture stirred at 60° C. for 6 hours
  2. 2
    workup.ADDITIONpoured onto water
  3. 3
    استخلاصextracted with ethyl acetate
  4. 4
    تجفيفdried over Na2SO4
  5. 5
    تركيزconcentrated under reduced pressure
  6. 6
    أخرىThe residue was purified

الإجراء التجريبي

Xantphos (32 mg), and Pd2(dba)3 (25 mg) were suspended in toluene (8 ml) and stirred under argon for 10 mins, then 2,2′-dichloro-[4,4′]-bipyridinyl (250 mg), 2-amino-1-methoxypropane (0.117 ml) and sodium tert-butoxide (150 mg) were added. The mixture stirred at 60° C. for 6 hours then cooled to room temp, poured onto water and extracted with ethyl acetate, dried over Na2SO4 and concentrated under reduced pressure. The residue was purified by passing the crude mixture down Kieselgel using a gradient of hexane and ethyl acetate as the eluent.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08389442B2uspto-grants-2013_03