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4-Hydroxypentanal synthesis

7synthesis methods
-

Yield:-

Reaction Conditions:

with hydrogenchloride in water; for 0.25 h;

Steps:

1.1

General procedure: To a solution of concentrated hydrochloric acid (62.5 mL, 0.71 mol) and water (750 mL) was added DHP(250 g, 3 mol) was added dropwise over 15 minutes to conduct acid treatment of DHP, 4-hydroxypentanal was obtained. At this time, the internal temperature rose from 21 ° C to 38 ° C. Thereafter, a 20% aqueous solution of sodium hydroxide (141.5 g, 0.71 mol)The mixture was added at 33 ° C. to adjust the pH to 10.5, and 5% aqueous hydrochloric acid (0.89 g) was added thereto to obtain pIt was adjusted to be H 7.9. Therein, (S) -1-methylbenzylamine ((S) -(+) - 1-phenylethylamine (PEA)) (360.1 g, 3 mol)At 23 ° C. and further added with sodium cyanide (NaCN) (145.72 g, 3 mol)Was added at the same temperature and stirred for 45 minutes. Thereafter, concentrated hydrochloric acid (309.6 g) was added at 5 ° C. to 18 ° C.Was added dropwise over 1 hour 30 minutes.

References:

JP2015/40200,2015,A Location in patent:Paragraph 0244; 0245; 0246