反应 #2195490

反应方程式

2-Thiophenecarbonylchloride

tert-butyl-1-piperazinecarboxylate

→

solids

收率 88.1%

4-(Thiophene-2-carbonyl)-piperazine-1-carboxylic acid tert-butyl ester

收率 88.1%

溶剂

pyridine

反应条件

后处理

1. 1
   过滤the precipitate was filtered
2. 2
   洗涤washed several times with water
3. 3
   其他dried

实验过程

2-Thiophenecarbonylchloride (2.04 g, 1.49 mL) was added to a solution of tert-butyl-1-piperazinecarboxylate (2.5 g, 13.4 mmol) and DMAP (20 mg) in pyridine (15 mL) at 0° C. under N2 atmosphere and stirred at room temperature for overnight. The mixture was poured into ice water, the precipitate was filtered, washed several times with water, and dried to yield white solids (3.5 g, 88%). Mp 76° C. 1H NMR (DMSO-d6): δ 1.42 (s, 12H), 3.40 (m, 4H), 3.61 (m, 4H), 7.12 (m, 1H), 7.43 (d, J=4.1 Hz, 1H), 7.77 (d, J=4.8 Hz, 1H). EIMS m/z 297 (M+1), 319 (M+23). Anal. (C14H20N2O3S) C, H, N.

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