morpholin-2-ylmethanol;hydrochloride

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: N-Benzyl-2-hydroxymethylmorpholine prepared in the same manner as described in Synthetic Communication, Vol. 10 (1), pages 59-73, 1980 (1.3 g) is subjected to hydrogenolysis in hydrogen chloride-containing ethanol in the same manner as described in Reference Example 15 to give 2-hydroxymethylmorpholine hydrochloride (1.3 g).

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: N-Benzyl-2-hydroxymethylmorpholine prepared in the same manner as described in Synthetic Communication, Vol. 10 (1), pages 59-73, 1980 (1.3 g) is subjected to hydrogenolysis in hydrogen chloride-containing ethanol in the same manner as described in Reference Example 15 to give 2-hydroxymethylmorpholine hydrochloride (1.3 g).

反応条件: temp:85.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Under argon, in a 500 ml round-bottomed flask equipped with a thermometer and a condenser, 10 g of (4-chloro-6-oxo-1,6-dihydropyrimidin-2-yl)acetic acid ethyl ester (example 25b, step 5b) and 9.6 g of morpholin-2-yl-methanol hydrochloride obtained previously are successively placed in 200 ml of DMSO and 16.1 ml of triethylamine. The reaction medium is heated for 22 h at 85° C. After returning to ambient temperature (20° C.), the reaction medium is poured into a saturated NaCl solution, and the mixture is extracted with 8×250 ml of ethyl acetate. The organic extracts are combined, dried over magnesium sulfate, filtered, and evaporated under reduced pressure. A solid is obtained which is slurried in diisopropyl ether containing 10% of methylene chloride. The solid is filtered off, and rinsed twice and then once with pentane. [4-(2-Hydroxymethylmorpholin-4-yl)-6-oxo-1,6-dihydropyrimidin-2-yl]acetic acid ethyl ester is isolated (1.9 g; yield=14%) in the form of a beige solid. obtained previously After returning to ambient temperature (20° C.) the mixture is extracted with 8×250 ml of ethyl acetate dried over magnesium sulfate filtered evaporated under reduced pressure A solid is obtained which The solid is filtered off rinsed twice

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In an autoclave under an argon atmosphere at ambient temperature (20° C.), 215 ml of methanol, 1.7 g of palladium hydroxide (12135-22-7), 12.4 g of (4-benzylmorpholin-2-yl)methanol and 15 ml of 4M HCl are successively placed in dioxane. After the autoclave has been closed, the reaction medium is placed under 6 bar of hydrogen at 25° C. for 24 h. The reaction medium is filtered through Clarcel, rinsed several times with methanol; the filtrate is concentrated under reduced pressure. Morpholin-2-ylmethanol hydrochloride (9.65 g) is isolated in the form of a yellow oil. at ambient temperature After the autoclave has been closed The reaction medium is filtered through Clarcel rinsed several times with methanol the filtrate is concentrated under reduced pressure

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: In an autoclave under an argon atmosphere at ambient temperature (20° C.), 215 ml of methanol, 1.7 g of palladium hydroxide (12135-22-7), 12.4 g of (4-benzylmorpholin-2-yl)methanol and 15 ml of 4M HCl are successively placed in dioxane. After the autoclave has been closed, the reaction medium is placed under 6 bar of hydrogen at 25° C. for 24 h. The reaction medium is filtered through Clarcel, rinsed several times with methanol; the filtrate is concentrated under reduced pressure. Morpholin-2-ylmethanol hydrochloride (9.65 g) is isolated in the form of a yellow oil. at ambient temperature After the autoclave has been closed The reaction medium is filtered through Clarcel rinsed several times with methanol the filtrate is concentrated under reduced pressure

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: N-Benzyl-2-hydroxymethylmorpholine prepared in the same manner as described in Synthetic Communication, Vol. 10 (1), pages 59-73, 1980 (1.3 g) is subjected to hydrogenolysis in hydrogen chloride-containing ethanol in the same manner as described in Reference Example 15 to give 2-hydroxymethylmorpholine hydrochloride (1.3 g).

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: N-Benzyl-2-hydroxymethylmorpholine prepared in the same manner as described in Synthetic Communication, Vol. 10 (1), pages 59-73, 1980 (1.3 g) is subjected to hydrogenolysis in hydrogen chloride-containing ethanol in the same manner as described in Reference Example 15 to give 2-hydroxymethylmorpholine hydrochloride (1.3 g).