反应详情

2-Methyl-benzothiazol-5-ol (2.5 g, 0.015 mol), cis-4-tert-butylcyclohexanol (2.84 g, 0.0182 mol), and Triphenylphosphine (4.76 g, 0.0182 mol) were combined in dry Toluene (100 mL, 1 mol) and stirred under nitrogen. Diisopropyl azodicarboxylate (3.6 mL, 0.018 mol) was added dropwise. The reaction was then stirred at RT overnight. Reaction was then concentrated to dryness and then residue was dissolved in DCM and 5 g of SiO2 was added. Solvent was removed under reduced pressure and resulting powder was loaded onto a 40 g column and purified via column chromatography using a gradient of 0-60% EtOAC/Hexanes.

1. stirringThe reaction was then stirred at RT overnight
2. customReaction
3. concentrationwas then concentrated to dryness
4. dissolutionresidue was dissolved in DCM
5. addition5 g of SiO2 was added
6. customSolvent was removed under reduced pressure
7. customresulting powder
8. custompurified via column chromatography