HRID43015
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
(S)-Ethyl-1-((2-(1-methylethylsulfonamido)-2,3-dihydro-1H-inden-5-yl)methyl)-5-(trifluoromethyl)-1H-pyrazole-4-carboxylate (0.026 mmol, 12 mg) was dissolved in THF (1 mL) and diisobutylaluminium hydride (0.304 mmol, 50 μL, 43.3 mg) added. After 15 min an additional 100 uL of DIBAL added and stirring continued for 30 min before the reaction was quenched with methanol. The mixture was concentrated then partitioned between DCM and Water. The aq. phase was acidified with 5N HCl and the phases mixed and separated using a hydrophobic frit. The organics were concentrated to dryness to give the desired compound as a clear film (10.6 mg, 0.025 mmol, 97%). MS (ESI): m/z [M+H]+ 418.2.
WORKUP
后处理
- customwas quenched with methanol
- concentrationThe mixture was concentrated
- customthen partitioned between DCM and Water
- additionthe phases mixed
- customseparated
- concentrationThe organics were concentrated to dryness