تفاعل #831002

ord-649e19fc45a4436093d1782ff4aea1cf

الكواشف

لا شيء

المذيبات

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    درجة الحرارةwas heated
  2. 2
    درجة الحرارةat reflux temperature for 24 hours
  3. 3
    درجة الحرارةOn cooling
  4. 4
    ترشيحthe mixture was filtered
  5. 5
    تركيزthe liltrate concentrated in vacuo
  6. 6
    أخرىThe residue on purification by flash chromatography on silica
  7. 7
    غسيلeluting with 5% v/v ethyl acetate/hexane

الإجراء التجريبي

A mixture of the product from step (i) above (4.91 g) and cuptic bromide (6.82 g) in ethyl acetate (45 ml) was heated at reflux temperature for 24 hours. On cooling, the mixture was filtered and the liltrate concentrated in vacuo. The residue on purification by flash chromatography on silica, eluting with 5% v/v ethyl acetate/hexane, gave methyl 4-bromoacetyl-2,6-di-tert-butylphenoxyacetate, 4.98 g, as an oil: NMR (d6DMSO) δ7.90 (2H, s), 4.92 (2H, s), 4.40 (2H, s), 3.76 (3H, s), 1.41 (18H, s).

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US05556977uspto-grants-1996_09