Method for preparing N-amino-3-azabicyclo[3,3,0]octane hydrochloride
A technology of octane hydrochloride and azabicycle, applied in the field of organic synthesis, can solve the problems of large environmental pollution, complicated operation, high difficulty and the like, and achieve the effect of reducing environmental pollution
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Embodiment 1
[0032] Add 68.5g (1.0mol) hydrazine monohydrochloride, 33.8g (0.33mol) concentrated hydrochloric acid, 43.4g (0.33mol) cis-cyclopentane-1,2-dimethanol, 100.0g water into a 500mL autoclave, 140 °C, react for 5 hours under the pressure of 2.2-5.6 atm. The reaction solution (containing hydrazine monohydrochloride and hydrazine dihydrochloride) was concentrated under reduced pressure, filtered, washed with methanol, and 54.2 g of crystals were precipitated. The mixture was titrated with 1N sodium hydroxide, and 42.2 g of hydrazine monohydrochloride was detected, with a recovery rate of 92.3%. The amount of water added is estimated in real time based on the viscosity of the feed.
[0033] The filtrate was concentrated, 6.1g of methanol was added, and crystallized at room temperature to obtain 29.2g of N-amino-3-azabicyclo[3,3,0]octane hydrochloride crystals, which were crystallized twice in the mother liquor to obtain N-amino- 8.6 g of 3-azabicyclo[3,3,0]octane hydrochloride crys...
Embodiment 2
[0036] Add 68.5g (1.0mol) hydrazine monohydrochloride, 33.8g (0.33mol) concentrated hydrochloric acid, 95.4g (0.33mol) cis-cyclopentane-1,2-dimethylsulfonate, and 100.0g water to a 500L reaction flask In, reflux reaction for 4 hours. The reaction solution (containing hydrazine monohydrochloride and hydrazine dihydrochloride) was concentrated under reduced pressure, washed with methanol, and 53.0 g of crystals were precipitated. The mixture was titrated with 1N sodium hydroxide to detect 41.0 g of hydrazine monohydrochloride, and the recovery rate was 90.3%.
[0037] Concentrate the filtrate again, then add 6.1g methanol, and crystallize at room temperature to obtain crystals of 29.4g N-amino-3-azabicyclo[3,3,0]octane hydrochloride, which is crystallized twice in the mother liquor to obtain N-amino-3-azabicyclo[3,3,0]octane hydrochloride crystal 8.8g, total yield 78.0%, content titration 100.1%, GC purity 99.5%.
[0038] 1 H NMR (400MHz, CDCl3): d = 7.0 (s, 2H), 3.16-3.41 (m...
Embodiment 3
[0040] Add 68.5g (1.0mol) hydrazine monohydrochloride, 33.8g (0.33mol) concentrated hydrochloric acid, 66.4.0g (0.33mol) cis-1,2-dichloromethyl-cyclopentane, and 100.0g water to a 500L reaction flask In, reflux reaction for 10 hours. The reaction solution (containing hydrazine monohydrochloride and hydrazine dihydrochloride) was concentrated under reduced pressure, washed with methanol, and 54.0 g of crystals were precipitated. The mixture was titrated with 1N sodium hydroxide to detect 42.1 g of hydrazine monohydrochloride, and the recovery rate was 92.2%.
[0041] Concentrate the filtrate again, then add 6.1g of methanol, and crystallize at room temperature to obtain 28.8g of N-amino-3-azabicyclo[3,3,0]octane hydrochloride crystals (101.87% by titration, 99.66% by GC) , secondary crystallization in the mother liquor to obtain 8.2 g of N-amino-3-azabicyclo[3,3,0]octane hydrochloride crystals (96.88% by titration, 94.53% by GC). The total yield is 75.4%, the content titratio...
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