report one,
Propylene oxide and ammonia water with a concentration of 95wt% in a molar ratio of 1:1.0 were respectively input into the mixer with a metering pump, and the temperature in the mixer was controlled to be 0°C and the pressure was 3.0MPa; the mixture was continuously fed into the microchannel for reaction In the reactor, the material reacts in the channel of the reaction section of the reactor, the temperature is 60 °C, the pressure is 3.0 MPa, and after staying for 0.1 s, it enters the cooling section of the microchannel reactor to rapidly cool down to terminate the reaction, the outlet temperature is 0 °C, and the temperature is 0 °C. The time is 2S, and the specific cooling rate is controlled at about 1800-2000°C/min. Then, the low boilers are removed through a stripping tower to obtain the product 1-amino-2-propanol with a content of 99.2%. In this embodiment, the microchannel reactor is specifically made of stainless steel, wherein the inner diameter of the microchannel is 0.05mm, and the length of the microchannel is 0.8m.
report two,
A preparation method of (S)-1-amino-2-propanol, specifically comprises the steps:
(1) Dissolve sodium tert-butoxide (230g, 2.39mol) in tetrahydrofuran (2L), slowly add trifluoroacetamide (226g, 2mol) under ice bath, stir for 30min; then add (S)- Propylene oxide (128 g, 2.2 mol) was naturally heated to room temperature, continued to stir for 10 h, and was stirred for 2 h at 35 °C; after the reaction, 2N (equivalent) hydrochloric acid was added dropwise to the system for a total of 1 L for neutralization, and then replenished 1 L of water was added, the layers were left to stand, the aqueous phase was extracted with dichloromethane, the organic phases were combined, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to obtain a total of 318 g of intermediate product I with a yield of 93%. 1H-NMR (CDCl3, 400MHz) of intermediate I: δ 1.08 (d, 3H), 3.37 (m, 2H), 4.0 (m, 1H), 7.12 (brs, 1H).
(2) The intermediate product I (310 g, 1.81 mol) obtained in step (1) was dissolved in methanol (1.5 L), 200 mL of water and potassium carbonate (550 g, 4 mol) were added, stirred at room temperature for 6 h, filtered, and concentrated to dryness, The obtained product was dissolved in dichloromethane, filtered to remove insoluble matter, dried over anhydrous sodium sulfate, concentrated, and distilled under reduced pressure to obtain the target product (S)-1-amino-2-propanol, a total of 122 g, with a yield of 90%. .
1H-NMR (CDCl3, 400MHz): δ 1.15 (d, 3H), 2.43 (dd, 1H), 2.64 (dd, 1H), 3.53-3.64 (m, 1H), 3.77 (brs, 3H). report three.
A preparation method of (R)-1-amino-2-propanol, specifically comprises the steps:
(1) Dissolve sodium tert-butoxide (300g, 3.12mol) in tetrahydrofuran (2L), slowly add trifluoroacetamide (294g, 2.6mol) under ice bath, stir for 30min; then add (R) under ice bath – Propylene oxide (166g, 2.96mol) was naturally heated to room temperature, continued to stir for 10h, and then stirred for 2h at 35°C; after the reaction, a total of 1.3L of 2N (equivalent) hydrochloric acid was added dropwise to the system for neutralization, Then 1.3 L of water was added, the layers were left to stand, the aqueous phase was extracted with dichloromethane, the organic phases were combined, dried over anhydrous sodium sulfate, and concentrated under reduced pressure to obtain a total of 423 g of intermediate product I with a yield of 95%.
1H-NMR (CDCl3, 400 MHz) of intermediate I: δ 1.07 (d, 3H), 3.36 (m, 2H), 3.99 (m, 1H), 7.11 (brs, 1H).
(2) Dissolve the intermediate product I (420g, 2.45mol) obtained in step (1) in methanol (2L), add 350mL of water and potassium carbonate (744g, 5.4mol), stir at room temperature for 6h, filter, and concentrate to dryness, The obtained product was dissolved in dichloromethane, filtered, insoluble matter was removed, dried over anhydrous sodium sulfate, concentrated, and distilled under reduced pressure to obtain the target product (R)-1-amino-2-propanol, a total of 171 g, with a yield of 93% .
1H-NMR (CDCl3, 400 MHz): δ 1.17 (d, 3H), 2.45 (dd, 1H), 2.66 (dd, 1H), 3.54-3.67 (m, 1H), 3.76 (brs, 3H).
