HRID1522578
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
CONDITIONS
反应条件
- 温度
- 0 °C
PROCEDURE
实验过程
7-Iodo-1H-pyrazolo[4,3-b]pyridine (1.5 g, 6.12 mmol) was dissolved in dry DMF (51.0 mL), cooled to 0° C. and NaH (0.245 g, 60% in oil, 6.12 mmol) was added. After 15 minutes and (2-(chloromethoxy)ethyl)trimethylsilane (1.080 mL, 6.12 mmol) was added and the mixture was warmed to room temperature over 2 hours then poured into ice water (350 mL) to give a solid which was filtered off. The filtrate was combined with dichloromethane and evaporated onto silica gel. Silica gel chromatography eluted with 0-5% MeOH in DCM gave 7-iodo-1-((2-(trimethylsilyl)ethoxy)methyl)-1H-pyrazolo[4,3-b]pyridine.
WORKUP
后处理
- temperaturethe mixture was warmed to room temperature over 2 hours
- customto give a solid which
- filtrationwas filtered off
- customevaporated onto silica gel
- washSilica gel chromatography eluted with 0-5% MeOH in DCM