반응 #2328976

ord-ddc890fef2474e41b5f817a96d24f359

용매

반응 조건

온도
15°CELSIUS
상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    workup.ADDITIONthe resulting solution was added dropwise at 15 to 16° C. over 40 minutes
  2. 2
    기타a sludge-like insoluble was removed by decantation
  3. 3
    세척the resulting organic layer was washed with in turn with 10% hydrochloric acid
  4. 4
    건조The organic layer was dried over anhydrous magnesium sulfate
  5. 5
    농축concentrated

실험 절차

5.7 g of lithium aluminum hydride was dispersed in 50 mL of THF and all of methyl trans-4-vinylcyclohexanecarboxylate was dissolved in 75 mL of THF and then the resulting solution was added dropwise at 15 to 16° C. over 40 minutes. After stirring at 10 to 20° C. for 30 minutes, water was slowly added. About 70 mL of 10% hydrochloric acid was added and a sludge-like insoluble was removed by decantation, and then the resulting organic layer was washed with in turn with 10% hydrochloric acid, a saturated sodium hydrogen carbonate solution, and saturated saline. The organic layer was dried over anhydrous magnesium sulfate and concentrated to obtain 26 g of (trans-4-vinylcyclohexyl)methanol.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US07670504B2uspto-grants-2010_03