反应详情

TBDMS-Cl (10.74 g, 71.2 mmol) and imidazole (5.38 g, 76.8 mmol) were added to a solution of 3-thiazol-2-yl-propan-1-ol (10.0 g 69.8 mmol) in THF (350 mL). Stirring was continued at rt overnight. The reaction mixture was partitioned between aq. sat. NH4Cl and Et2O. The aq. layer was extracted again with Et2O, the combined org. extracts were dried over MgSO4, filtered, and solvents were removed in vacuo. Purification of the crude by FC(CH2Cl2/MeOH 95:5) yielded the title compound as an orange oil (13.00 g, 72%). LC-MS: tR=1.05 min, ES+: 258.24.

1. customThe reaction mixture was partitioned between aq. sat. NH4Cl and Et2O
2. extractionThe aq. layer was extracted again with Et2O
3. dry with materialextracts were dried over MgSO4
4. filtrationfiltered
5. customsolvents were removed in vacuo
6. customPurification of the crude by FC(CH2Cl2/MeOH 95:5)