HRID734800
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
1.14 g (3.61 mmol) of TBAF was added at RT to a solution of 1.25 g (3.61 mmol) of 2-[(tert-butyldimethylsilanyl)ethynyl]-5-(4-chlorophenyl)-3-fluoropyridine in 30 mL of DCM and the mixture was stirred for 2 hours. The organic phase was washed with water, dried over sodium sulfate, and evaporated down in vacuo. The residue was stirred with PE, the precipitate was filtered off, washed with PE, and dried in the air. Yield: 0.72 g (86% of theoretical); C13H7ClFN (M=231.653); calc.: molpeak (M+H)+: 232/234 (Cl); found: molpeak (M+H)+: 232/234 (Cl); HPLC-MS: 5.81 minutes (method B).
WORKUP
后处理
- washThe organic phase was washed with water
- dry with materialdried over sodium sulfate
- customevaporated down in vacuo
- stirringThe residue was stirred with PE
- filtrationthe precipitate was filtered off
- washwashed with PE
- customdried in the air
- custom5.81 minutes (method B)