تفاعل #1138940

ord-2cf0b8277a6244cd98ca38cb8d1116c1

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGThe resulting mixture is stirred at RT for an additional 2 h
  2. 2
    استخلاصThe mixture is extracted with ethyl acetate (2×100 mL)
  3. 3
    غسيلThe combined organic layers are washed with brine
  4. 4
    تجفيفdried over Na2SO4
  5. 5
    ترشيحfiltered
  6. 6
    تركيزThe filtrate is concentrated in vacuo

الإجراء التجريبي

To a stirred solution of phenylmethanol (3.35 g, 31 mmol, 1.2 eq) in THF (80 mL), NaH (60% dispersion in mineral oil, 1.34 g, 33.5 mmol, 1.3 eq) is added in portions. The resulting mixture is stirred at RT for 30 min and then 8-bromo-6-chloroimidazo[1,2-b]pyridazine (D-3) (6 g, 25.8 mmol, 1.0 eq) is added. The resulting mixture is stirred at RT for an additional 2 h and then poured into water (30 mL). The mixture is extracted with ethyl acetate (2×100 mL). The combined organic layers are washed with brine, dried over Na2SO4 and filtered. The filtrate is concentrated in vacuo to afford the product, 8-(benzyloxy)-6-chloroimidazo[1,2-b]pyridazine (D-4).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US09388183B2uspto-grants-2016_07