Propylene oxide as well as ammonia water with a focus of 95wt% are input into the mixer with a metering pump at a molar ratio of 1:1.0, and also the temperature in the mixer is regulated at 0 ° C and also the stress at 3.0 MPa; the blended solution is continually fed right into the microchannel for reaction In the reactor, the product responds in the network of the response section of the activator. The temperature level is 60 ° C and the stress is 3.0 MPa. The moment is 2S, and also the particular air conditioning rate is controlled at concerning 1800-2000 ° C/min. After that the reduced central heating boilers are gotten rid of through a stripping tower to obtain the product Isopropanolamine with a material of 99.2%. In this embodiment, the microchannel reactor is particularly made from stainless steel, where the internal size of the microchannel is 0.05 mm, and the size of the microchannel is 0.8 m.
A preparation approach for Isopropanolamine, specifically making up the steps of:
( 1) Liquify sodium tert-butoxide (230g, 2.39 mol) in tetrahydrofuran (2L), slowly add trifluoroacetamide (226g, 2mol) under ice-cooling, stir for 30min; after that include (S)- Propylene oxide (128g, 2.2 mol), naturally heated up to area temperature level, remained to stir for 10h, after that mixed for an additional 2h at 35 ° C; after the response, included 1L of 2N (normal focus) hydrochloric acid dropwise to the system for neutralization, and added Include 1L of water, stand to separate the layers, essence the liquid phase with dichloromethane, integrate the natural stages, completely dry over anhydrous salt sulfate, and concentrate under reduced pressure to obtain 318 g of intermediate item I, with a yield of 93%. 1H-NMR (CDCl3, 400MHz) of intermediate product I: δ1.08 (d, 3H), 3.37 (m, 2H), 4.0 (m, 1H), 7.12 (brs, 1H).
( 2) Liquify the intermediate item I (310g, 1.81 mol) gotten in step (1) in methanol (1.5 L), add 200mL of water and also potassium carbonate (550g, 4mol), mix at area temperature level for 6h, filter, and also concentrate to dry skin. The obtained product was dissolved in dichloromethane, filteringed system to get rid of insoluble issue, dried over anhydrous salt sulfate, concentrated, and distilled under lowered pressure to obtain 122 g of the target item Isopropanolamine with a return of 90%.
1H-NMR (CDCl3, 400MHz): δ1.15 (d, 3H), 2.43 (dd, 1H), 2.64 (dd, 1H), 3.53-3.64 (m, 1H), 3.77 (brs, 3H).
A preparation technique for Isopropanolamine, particularly consisting of the steps of:
( 1) Liquify salt tert-butoxide (300g, 3.12 mol) in tetrahydrofuran (2L), gradually include trifluoroacetamide (294g, 2.6 mol) under ice-cooling, mix for 30min; after that add (R) under ice-cooling – Propylene oxide (166g, 2.96 mol), naturally warming up to area temperature, continue to mix the response for 10h, and then stir the response for 2h at 35 ° C; after the reaction, include an overall of 1.3 L of 2N (typical concentration) hydrochloric acid to the system for neutralization, 1.3 L of water was added, as well as the layers were enabled to stand. The liquid phase was extracted with dichloromethane. The organic stages were combined, dried over anhydrous salt sulfate, as well as focused under lowered stress to get 423 g of intermediate product I with a return of 95%.
1H-NMR (CDCl3, 400MHz) of intermediate product I: δ1.07 (d, 3H), 3.36 (m, 2H), 3.99 (m, 1H), 7.11 (brs, 1H).
( 2) Liquify the intermediate product I (420g, 2.45 mol) obtained symphonious (1) in methanol (2L), include 350mL of water and also potassium carbonate (744g, 5.4 mol), stir at room temperature level for 6h, filter, and also concentrate to dry skin. The item acquired was dissolved in dichloromethane, filtered to remove insoluble issue, dried over anhydrous sodium sulfate, focused, and distilled under minimized pressure to acquire an overall of 171 g of the target product (R)-1-amino-2-propanol, with a yield of 93%.
1H-NMR (CDCl3, 400MHz): δ1.17 (d, 3H), 2.45 (dd, 1H), 2.66 (dd, 1H), 3.54-3.67 (m, 1H), 3.76 (brs, 3H).
