HRID1907837
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
To a solution of XXVIII (475 mg, 1.28 mmol) in dry THF (3 mL) was added methylhydrazine (273 μL, 5.13 mmol). The resulting solution was stirred at room temperature for 18 hrs, the solvent removed in vacuo and the residue taken up in CH2Cl2. The CH2Cl2 solution was washed with H2O, dried over MgSO4, filtered and CH2Cl2 evaporated in vacuo to afford XIX as a yellow oil (0.43 g, 88%): 1H NMR (DMSO-d6) δ 7.48 (app s, 2H), 7.47 (app s, 2H), 5.84 (s, 1H), 4.86 (bs, 2H), 3.42 (s, 3H), 3.19 (s, 3H); ESI/MS 381 (M+H), 366 (M−CH3).
WORKUP
后处理
- customthe solvent removed in vacuo
- washThe CH2Cl2 solution was washed with H2O
- dry with materialdried over MgSO4
- filtrationfiltered
- customCH2Cl2 evaporated in vacuo