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CAS No. : | 475-11-6 | MDL No. : | MFCD00011565 |
Formula : | C6H11NO2 | Boiling Point : | No data available |
Linear Structure Formula : | - | InChI Key : | - |
M.W : | 129.16 | Pubchem ID : | - |
Synonyms : |
|
Chemical Name : | H-N-Me-Pro-OH |
Signal Word: | Warning | Class: | |
Precautionary Statements: | P261-P280-P305+P351+P338 | UN#: | |
Hazard Statements: | H302-H315-H319-H332-H335 | Packing Group: | |
GHS Pictogram: |
* All experimental methods are cited from the reference, please refer to the original source for details. We do not guarantee the accuracy of the content in the reference.
Yield | Reaction Conditions | Operation in experiment |
---|---|---|
92% | With palladium 10% on activated carbon; hydrogen; In methanol; water; | General procedure: L-Proline(2.0 g, 17.4 mmol) was dissolved in methanol (20 mL) and40 % aqueous formaldehyde (1.4 mL, 19.1 mmol) wasadded to this solution. Next, 10 % Pd/C catalyst (500 mg)was added to the reaction mixture and the resulting slurrywas stirred in hydrogen overnight. The slurry was then filtered through a Celite pad to remove the catalyst. Thepad was washed with methanol and the combined filtrateswere concentrated under reduced pressure. The residue wasdissolved in ethanol/benzene (1:1, 100 mL) and concentratedsecond time to provide a solid that was re-crystallizedin methanol/diethyl ether. In this way Nmethylproline7a was isolated as fine needles (2.1 g, 92 %yield); mp 109-111C; 1H NMR (D2O, 300 MHz):delta = 3.95-3.90 (1H, m, CH2 (CH2)2CHNCH3), 3.24-3.15(2H, m, CH2 (CH2)2CHNCH3), 2.97 (3H, s, CH2 (CH2)2CHNCH3), 2.22-2.01 (4H, m, CH2 (CH2)2CHNCH3); ESI-MS (m/z):130.2 [M + H] +(100). |
89% | With palladium 10% on activated carbon; hydrogen; In methanol; at 20℃; for 24h; | L-proline (4.0 g, 34.8 mmol)Soluble in methanol (40mL),40% aqueous formaldehyde solution (2.8 mL, 38.2 mmol) was added in orderAnd 10% Pd on carbon (1g), addition, hydrogenation,Reaction at room temperature for 24 hours,After the reaction is complete, filterThe mother liquor was concentrated and dried to give 4g of a white solid with a yield of 89%.That is, N-methyl-L-proline (compound b). |
88% | With sodium dihydrogenphosphate; zinc; In water; at 30℃; for 48h; | The vigorously stirred suspension of zinc dust(6.50 g; 100 mmol), L-proline (5.57 g; 50 mmol) and NaH2PO4 (11.90 g; 100 mmol) in water (22 mL) was treated with 35% aq. formaldehyde (2.10 mL).Stirring was continued for 48 h at 30C. The suspension was discarded, the filtrate was neutralized with2 M aq. ammonia to pH 8, concentrated under vacuum,the solid residue was dissolved in small amount of water and lyophilized. Dry residue was extracted with hot mixture of benzene-ethanol (1 : 1, v/v).Collected extracts were evaporated to dryness and then recrystallized from the mixture methanol/ether affording L-N-methylproline (1) (5.68 g; yield 88%)as white crystals m.p. 115-120C, lit. (12) m.p.115-116C. |
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