HRID1628110
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
- 65 °C
PROCEDURE
实验过程
To a solution of (E)-ethyl 3-(1-cyclohexyl-6-tosyl-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-3-yl)acrylate (0.064 g, 0.13 mmol) in 1,4-dioxane (5 mL) was added aqueous NaOH (2 N, 1.30 mL, 2.60 mmol). The mixture was heated to about 65° C. After about 15 h, the mixture was cooled to rt and the pH of the reaction mixture was adjusted to about pH=1 with concentrated HCl. The mixture was partially concentrated in vacuo and the precipitate was collected by filtration and dried in vacuo to provide (E)-3-(1-cyclohexyl-6H-imidazo[1,5-a]pyrrolo[2,3-e]pyrazin-3-yl)acrylic acid (0.015 g, 37%): LC/MS (Table 2, Method a) Rt=1.85 min; MS m/z: 311 (M+H)+. Syk IC50=B.
WORKUP
后处理
- temperaturethe mixture was cooled to rt
- concentrationThe mixture was partially concentrated in vacuo
- filtrationthe precipitate was collected by filtration
- customdried in vacuo