反应详情

Step 2 To a stirred solution of 1-tert-butyl 1-ethyl cyclopropane-1,1-dicarboxylate (0.5 g, 2.33 mmol) in THF (11.7 mL) at −78° C. was added lithium tri-tert-butoxyaluminum hydride solution (11.7 mL, 11.7 mmol) dropwise. The mixture was warmed to room temperature and stirred overnight before it was quenched at 0° C. by the addition of a saturated solution of potassium sodium tartrate. EtOAc was added the phases were separated and the aqueous phase was extracted into EtOAc (×2). Combined organic extracts were dried (Na2SO4), filtered and concentrated providing tert-butyl 1-(hydroxymethyl)-cyclopropane-1-carboxylate which was used without further purification, 0.438 g.

1. customwas quenched at 0° C. by the addition of a saturated solution of potassium sodium tartrate
2. additionEtOAc was added the phases
3. customwere separated
4. extractionthe aqueous phase was extracted into EtOAc (×2)
5. dry with materialCombined organic extracts were dried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated