反応 #2195490

反応方程式

2-Thiophenecarbonylchloride

tert-butyl-1-piperazinecarboxylate

→

solids

収率 88.1%

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

収率 88.1%

溶媒

pyridine

反応条件

後処理

1. 1
   ろ過the precipitate was filtered
2. 2
   洗浄washed several times with water
3. 3
   その他dried

実験手順

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.

出典