反应详情

To 0.6 mmol 5-cyclopropanesulfonyl-2-hydroxy-benzoic acid methyl ester, 3.7 mmol 2-propanol and 0.9 mmol diphenyl-2-pyridylphosphine in 8 ml THF was added 0.9 mmol di-tert-butyl azodicarboxylate, and the mixture was stirred at RT for 3 h. 4 mmol 5 M aq NaOH solution was then added, and the mixture heated at 60° C. for 1 h. The mixture was then concentrated in vacuo. The residue was resuspended in ethyl acetate and washed twice with 1 M aq NaOH solution. The combined aqueous phases were then acidified to pH 1 by addition of 25% aq HCl and extracted three times with ethyl acetate. The combined organic extracts were then dried with Na2SO4, and concentrated in vacuo to afford the title compound. MS (m/e): 282.9 ([M−H]−, 100%)

1. temperaturethe mixture heated at 60° C. for 1 h
2. concentrationThe mixture was then concentrated in vacuo
3. washwashed twice with 1 M aq NaOH solution
4. additionThe combined aqueous phases were then acidified to pH 1 by addition of 25% aq HCl
5. extractionextracted three times with ethyl acetate
6. dry with materialThe combined organic extracts were then dried with Na2SO4
7. concentrationconcentrated in vacuo