تفاعل #2350733

ord-9e61a3f015f24ec4b09636b88de9df82

الكواشف

لا شيء

ظروف التفاعل

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

المعالجة

  1. 1
    workup.STIRRINGthe mixture is stirred for 15 minutes at room temperature
  2. 2
    أخرىthe layers are separated
  3. 3
    استخلاصthe aqueous layer is extracted with ethyl acetate (3×)
  4. 4
    تجفيفThe combined organic layers are dried over sodium sulphate
  5. 5
    ترشيحfiltered
  6. 6
    تركيزconcentrated

الإجراء التجريبي

To a stirred solution of 60 mmol NaOH in 50 ml N,N-dimethyl formamide is progressively added 50 mmol 2,6-diiodo-4-(4-methoxy-butyl)-pyridin-3-ol. The reaction mixture is stirred for 30 minutes and then cooled to 0° C. 60 mmol methyl iodide are added and the mixture is stirred for 15 minutes at room temperature. Water and ethyl acetate are added to the mixture, the layers are separated and the aqueous layer is extracted with ethyl acetate (3×). The combined organic layers are dried over sodium sulphate, filtered and concentrated. The title compound is obtained from the residue by means of flash chromatography (SiO2 60 F) and identified based on its Rf value.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07851634B2uspto-grants-2010_12