HRID2427270
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
Combine crude (S)-{7-cyano-4-[2-(1,3-dioxo-1,3-dihydro-isoindol-2-yl)-pyridin-3-ylmethyl]-1,2,3,4-tetrahydro-cyclopenta[b]indol-2-yl}-carbamic acid isopropyl ester (2.12 mmol, 1100 mg crude material) in a mixture of THF (22 mL) and ethanol (4 mL) and stir for 15 min. Add hydrazine hydrate 0.5 mL, 10 mmol) and stir the mixture at room temperature for 18 h. Vacuum filter the crude reaction and wash the solid with THF (50 mL). Collect the filtrate and remove the solvent under vacuum. Purify the resulting residue by silica gel chromatography (50-100% ethyl acetate/CH2Cl2) to provide 110 mg (13%) of the title compound. MS (m/z): 390 (M+1).
WORKUP
后处理
- filtrationVacuum filter the crude
- customreaction
- washwash the solid with THF (50 mL)
- customCollect the filtrate
- customremove the solvent under vacuum
- customPurify the resulting residue by silica gel chromatography (50-100% ethyl acetate/CH2Cl2)