Method for preparing isothiocyanate
A technology of isothiocyanate and acid-binding agent, which is applied in the field of preparation of isothiocyanate, can solve the problems of inconvenient acquisition of formamide and sulfonyl halide, low yield of target product, cumbersome operation process, etc., and achieve separation The effect of convenient purification, short reaction time, and easy availability of reaction raw materials
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[0023] Example 1
[0024] Weigh phenoxysulfuryl chloride (1 mmol) and sodium hydroxide (1 mmol) and add them to a single-neck flask containing dichloromethane (5 mL). 0 Stir at C. Then weigh benzylamine (1 mmol) and dissolve it in dichloromethane (1 mL), add dropwise to the above flask, and stir and react for 30 hours. The reaction was stopped, water (10 mL) and dichloromethane (15 mL) were added, and the organic phase was extracted and separated. The aqueous phase was extracted with dichloromethane (15 mL). The organic phases were combined and washed with saturated brine (15 mL). Dry with anhydrous sodium sulfate. After separation by column chromatography (ethyl acetate: petroleum ether = 1:5), benzyl isothiocyanate was obtained with a yield of 80%.
[0025] 1 H NMR (500 MHz, CDCl 3 ) δ : 7.39 (t, J = 7.0 Hz, 2H, ArH), 7.35 (d, J = 7.0 Hz, 1H, ArH), 7.31 (d, J = 7.0 Hz, 2H, ArH), 4.71 (s, 2H, NCH 2 ). 13 C NMR (125 MHz, CDCl 3 ) δ : 134.3, 129.0 (N=C=S), 128.4, 126.8, 48.7...
Example Embodiment
[0026] Example 2
[0027] Weigh phenoxysulfuryl chloride (3 mmol) and sodium hydroxide (10 mmol), add them to a single-neck flask containing xylene (5 mL), and stir at room temperature. Then weigh benzylamine (1 mmol) dissolved in xylene (1 mL) and add it dropwise to the above flask. 0 The reaction was stirred at C for 1 hour. The reaction was stopped, the solvent was evaporated under reduced pressure, water (10 mL) and dichloromethane (15 mL) were added, the organic phase was extracted and separated, the aqueous phase was extracted with dichloromethane (15 mL), the organic phases were combined, and saturated salt was used. Wash with water (15 mL) and dry with anhydrous sodium sulfate. After separation by column chromatography (ethyl acetate: petroleum ether = 1:5), benzyl isothiocyanate was obtained with a yield of 86%.
Example Embodiment
[0028] Example 3
[0029] Weigh phenoxysulfuryl chloride (1.2 mmol) and sodium hydroxide (3 mmol), add them to a single-neck flask containing dichloromethane (5 mL), and stir in an ice bath. Then weigh benzylamine (1 mmol) dissolved in dichloromethane (1 mL), add dropwise to the above flask, keep the temperature at 0~5℃; remove the ice bath after 1 hour, +30 0 The reaction was stirred at C for 10 hours. The reaction was stopped, water (10 mL) and dichloromethane (15 mL) were added, and the organic phase was extracted and separated. The aqueous phase was extracted with dichloromethane (15 mL). The organic phases were combined and washed with saturated brine (15 mL). Dry with anhydrous sodium sulfate. After column chromatography (ethyl acetate: petroleum ether = 1:5), benzyl isothiocyanate was obtained with a yield of 95%.
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