반응 #1143013

반응 방정식

2-(2-methoxyethoxyl)ethanamine

1,1′-thiocarbonyldiimidazole

water

→

1-isothiocyanato-2-(2-methoxyethoxyl)ethane

수율 61.2%

용매

DMF

DMF

반응 조건

후처리

1. 1
   추출extracted with Et2O (70 mL)
2. 2
   세척The Et2O layer was washed with water
3. 3
   건조dried over Na2SO4
4. 4
   여과filtered
5. 5
   농축The filtrate was concentrated in vacuo (325 torr, bath temp: 24° C.)

실험 절차

To a solution of 2-(2-methoxyethoxyl)ethanamine (0.820 g, 6.88 mmol) in DMF (69 mL) at 0° C. was added dropwise a solution of 1,1′-thiocarbonyldiimidazole (1.349 g, 7.57 mmol) in 21 mL of DMF. The mixture was warmed to RT and stirred for 90 min. The mixture was poured into water (130 mL) and extracted with Et2O (70 mL). The Et2O layer was washed with water, dried over Na2SO4, and filtered. The filtrate was concentrated in vacuo (325 torr, bath temp: 24° C.) to afford 1-isothiocyanato-2-(2-methoxyethoxyl)ethane (0.678 g, 4.21 mmol, 61% yield) as a yellow oil. The crude material was used in next step.

출처