تفاعل #57060

ord-4543cd007d8f4a4d963bcad71a899e4c

الكواشف

لا شيء

ظروف التفاعل

الظروف التفصيلية
See reaction.notes.procedure_details.

المعالجة

  1. 1
    workup.ADDITIONAfter addition
  2. 2
    أخرىthe cold bath was removed
  3. 3
    workup.STIRRINGThe mixture was stirred over night
  4. 4
    استخلاصthe mixture was extracted with ethyl acetate
  5. 5
    غسيلThe combined organic phase was washed with water and brine

الإجراء التجريبي

To a solution of LDA (30 mL, 2.0M, 60 mmol) in THF/heptane/ethylbenzene and anhydrous THF (30 mL) at 0° C. was added cyclobutane carboxylic acid (3.0 g, 30 mmol) dropwise. After addition was complete, the cold bath was removed, the reaction mixture was stirred at room temperature for 2 hr. Neat n-BuI (3.41 mL, 30 mmol) was added dropwise at room temperature. The mixture was stirred over night. To the mixture was added 2N HCl and the mixture was extracted with ethyl acetate. The combined organic phase was washed with water and brine to afford the title compound as a light yellow oil (quantitative), which was used in the next step without purification.

المصدر

DOI: 10.6084/m9.figshare.5104873.v1براءة الاختراع: US07419999B2uspto-grants-2008_09