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
- 50 °C
PROCEDURE
实验过程
A mixture of (2S)-methyl 2-(7-(4-allyl-5-chloro-3,4-dihydro-2H-benzo[b][1,4]oxazin-6-yl)-2-(3′-(allyloxy)-[1,1′-biphenyl]-3-yl)-5-methylpyrazolo[1,5-a]pyrimidin-6-yl)-2-(tert-butoxy)acetate (40 mg, 0.058 mmol) and Hoveyda-Grubbs 2nd generation catalyst (4.90 mg, 5.77 μmol) catalyst in DCE (2 mL) was heated at 50° C. for 5 h. Mixture was then cooled to room temp and concentrated under reduced pressure. Mixture was then treated with 1N NaOH (0.173 mL, 0.173 mmol) in MeOH (2.0 mL) at 50° C. for 3 h. Mixture was then cooled to room temp and purified by prep-HPLC to afford desired product (10 mg, 0.015 mmol, 26.6% yield) as inseparable mixture of cis and trans isomers. Used as is in the next step without further purification. LCMS (M+H)=651.3.
WORKUP
后处理
- temperatureMixture was then cooled to room temp
- concentrationconcentrated under reduced pressure
- temperatureMixture was then cooled to room temp
- custompurified by prep-HPLC