HRID592450

反应详情

EQUATION

反应方程式

HRID 592450 的结构方程式

PROCEDURE

实验过程

A solution of 1-(2-iodophenyl)cyclobutanecarboxylic acid A52 (425 mg, 1.41 mmol) in MeOH (25 mL) and conc. H2SO4 (1.0 mL) was stirred at 60° C. overnight. The volatiles were removed in vacuo and the resulting residue diluted in EtOAc (50 mL) and sat. soln. Na2CO3 (50 mL). The aqueous layer was extracted with EtOAc (3×50 mL), the combined organic fractions were dried (MgSO4) and the volatiles removed in vacuo to give the title compound A53 as a clear oil (361 mg, 81%). LCMS-A: rt 7.020 min; m/z 317 [M+H]+.

WORKUP

后处理

  1. customThe volatiles were removed in vacuo
  2. additionthe resulting residue diluted in EtOAc (50 mL)
  3. extractionThe aqueous layer was extracted with EtOAc (3×50 mL)
  4. dry with materialthe combined organic fractions were dried (MgSO4)
  5. customthe volatiles removed in vacuo