A kind of preparation method of n-benzyl hydroxylamine and its hydrochloride
A technology of benzylhydroxylamine hydrochloride and benzylhydroxylamine is applied in the field of preparation of N-benzylhydroxylamine and its hydrochloride, and can solve the problems of lack of good improvement, complicated procedures, low yield and the like, and achieves The effect of mild reaction, simple conditions and low price
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Embodiment 1
[0012] 1. Oximation
[0013] In a 1-liter clean four-neck flask, add 600 ml of water, 72 g (1.02 moles) of hydroxylamine hydrochloride, stir and dissolve, add 165 g of 25% NaOH solution, and cool the ice water to about 20°C, between 20-30°C 108 g (1.02 mol) of benzaldehyde was added dropwise. After the addition was complete, it was stirred at room temperature for 1 hour. Stand for 30 minutes to separate the layers, separate the lower layer of oil, wash once with water, anhydrous MgSO 4 After drying and filtering, about 102 grams of brown oily benzaldoxime was obtained, with a yield of about 85%.
[0014] 2. Reduction and Salt Formation
[0015] In a 1-liter clean and dry four-neck flask, add 108 grams (0.9 moles) of benzaldehyde oxime, 600 milliliters of anhydrous methanol, and drop 2 drops of methyl orange indicator, cool the ice water to below 20 ° C, add dropwise HCl- methanol solution to keep the solution pink, while slowly adding 37.2 g (0.6 mol) NaBH 3 CN, heat will ...
Embodiment 2
[0017] 1. Oximation
[0018] In a 1-liter clean four-necked flask, add 600 ml of water, 72 g (1.02 moles) of hydroxylamine hydrochloride, stir and dissolve, add 156 g of 25% NaOH solution, and cool the ice water to about 20°C, between 20-30°C 108 g (1.02 mol) of benzaldehyde was added dropwise. After the addition was complete, it was stirred at room temperature for 1 hour. Stand for 30 minutes to separate the layers, separate the lower layer of oil, wash once with water, anhydrous MgSO 4 After drying and filtering, about 108 grams of brown oily benzaldoxime was obtained, with a yield of about 90%.
[0019] 2. Reduction and salt formation
[0020] In a 1-liter clean and dry four-neck flask, add 108 grams (0.9 moles) of benzaldehyde oxime, 600 milliliters of anhydrous methanol, and drop 2 drops of methyl orange indicator, cool the ice water to below 20 ° C, add dropwise HCl- methanol solution to keep the solution pink, while slowly adding 37.2 g (0.6 mol) NaBH 3 CN, heat wil...
Embodiment 3
[0022] 1. Preparation of benzaldoxime
[0023] In a 1-liter clean four-necked flask, add 600 milliliters of water, 72 grams (1.02 moles) of hydroxylamine hydrochloride, stir and dissolve, add 156 grams of 25% NaOH solution, and cool the ice water to about 20°C. 108 g (1.02 moles) of benzaldehyde was added dropwise. After the addition was completed, it was stirred at room temperature for 1 hour. Stand for 30 minutes to separate the layers, separate the lower layer of oil, wash once with water, anhydrous MgSO 4 Dry and filter to obtain about 108 grams of brown oily benzaldoxime, with a yield of about 90%, which is set aside.
[0024] 2. Preparation of N-benzylhydroxylamine
[0025] In a 1-liter clean and dry four-neck flask, add 108 grams (0.9 moles) of benzaldehyde oxime, 600 milliliters of anhydrous methanol, and drop 2 drops of methyl orange indicator, cool the ice water to below 20 ° C, add HCl dropwise - Methanol solution to keep the solution pink while slowly adding 37....
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