تفاعل #1553216

ord-58342708b902474b9faef8ce39a3b550

الكواشف

لا شيء

ظروف التفاعل

درجة الحرارة
0°CELSIUS
الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.STIRRINGThe mixture was stirred for 2 hours at 0° C
  2. 2
    أخرىThe reaction was quenched with water
  3. 3
    استخلاصextracted with EtOAc
  4. 4
    غسيلThe combined organic phase was washed with brine
  5. 5
    تجفيفdried over anhydrous Na2SO4
  6. 6
    تركيزconcentrated
  7. 7
    أخرىThe residue was purified by silica gel column chromatograph

الإجراء التجريبي

To a mixture of CH3OCH2PPh3I (8.9 g, 26 mmol) in THF (80 mL) was added a solution of NaHMDS in THF (2.0M, 13 mL, 26 mmol)) at 0° C. The mixture was stirred 1 hour at 0° C. Then a solution of 1-Oxoindane-5-carbonitrile (2.0 g, 13 mmol) in THF (10 mL) was added. The mixture was stirred for 2 hours at 0° C. The reaction was quenched with water and extracted with EtOAc. The combined organic phase was washed with brine, dried over anhydrous Na2SO4 and concentrated. The residue was purified by silica gel column chromatograph to give the title compound. MS m/z: 186 [M+1]+.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US08999990B2uspto-grants-2015_04