HRID717778
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
- 95 °C
PROCEDURE
实验过程
4-Nitroso-3,4-dihydro-2H-benzo[1,4]thiazine (1 g, 5.55 mmol) was dissolved in acetic acid (25 mL) and N-Me- piperidone (753 mg, 6.66 mmol) and zinc dust (1.8 g, 27.77 mmol) was added portionwise at RT. The reaction mixture was heated at 95° C. for 2 h. After completion of reaction, the mixture was basified with NaHCO3 and extracted with EtOAc, dried over sodium sulfate and concentrated under vacuum to obtain product. 1H NMR (CD3OD, Formate Salt): d (ppm): 7.20 (d, 1H), 6.98 (t, 1H), 6.90 (d, 1H), 4.32 (t, 2H), 4.28 (s, 2H), 3.50 (t, 2H), 3.30 (m, 2H), 3.10 (t, 2H), 2.98 (s, 3H).
WORKUP
后处理
- customAfter completion of reaction
- extractionextracted with EtOAc
- dry with materialdried over sodium sulfate
- concentrationconcentrated under vacuum
- customto obtain product